Month: May 2021

Application of 3485-84-5, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 3485-84-5, name is N-Vinylphthalimide belongs to indolines-derivatives compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In a sealed tube under argon atmosphere, were introducedcompound 4 (4.74 g, 20 mmol), DMF (20 mL), triethylamine(11.16 mL, 80 mmol), palladium diacetate (225 mg, 1 mmol), tri(otolyl)-phosphine (609 mg, 2 mmol) and N-vinylphthalimide (5.20 g,30 mmol). The mixturewas stirred at 110 C for 3 h and hydrolyzed.The formed solid was solubilized in CH2Cl2, washed with water andbrine, dried over MgSO4 and evaporated under reduced pressure.The crude productwas recrystallized from acetonitrile to afford 7 asa white solid (91% yield); Mp 199-200 C; 1H NMR (300 MHz,CDCl3):delta 8.49 (d, 1H, 15 Hz), 8.25 (d, 1H, 15 Hz), 8.00 (d, 1H, 9.0 Hz),7.92 (m, 2H), 7.81 (d, 1H, 7.8 Hz), 7.76 (m, 2H), 7.65 (d, 1H, 7.8 Hz),7.38 (t, 1H, 7.8 Hz), 6.96 (d, 1H, 9.0 Hz), 4.23 (s, 3H); IR (upsilon, cm-1, KBr):1715 (C=O); MS (APCI, pos. 30 V) m/z: [M+H]+, 331.34. HRMS(ESI+): m/z = calcd. for C20H15N2O3 [M+H]+ 331.10772 found:331.10606.

The synthetic route of N-Vinylphthalimide has been constantly updated, and we look forward to future research findings.

Related Products of 552330-86-6, These common heterocyclic compound, 552330-86-6, name is 5-Bromoisoindolin-1-one, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

5-Bromo-2,3-dihydro-isoindol-l-one (leq) was added to a solution of benzyl bromide (l . l eq) and K2CO3 (2eq) in DMF under N2. The mixture was stirred at rt for 16 hrs. Reaction was diluted in water and the compound precipitated. The solid was filtered and dried under reduced pressure. Compound was used in the next step without further purification.

The synthetic route of 552330-86-6 has been constantly updated, and we look forward to future research findings.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 667463-64-1, name is 6-Bromo-1-methylindoline-2,3-dione, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 6-Bromo-1-methylindoline-2,3-dione

I-3.1 (397 mg, 1.65 mmol) and hydrazine hydrate (1 mL, 20.6 mmol) are heated to 100 C. for 1 h and at 125 C. for 1 h. To the cool reaction mixture DCM and water are added and the aqueous layer extracted twice with DCM. The combined organic layers are washed with brine, dried, concentrated and the residue purified via column chromatography (using solvent mixture cyclohexane/EA=3:1). Yield 65%. m/z 226 [M+H]+, m/z 224 [M+H]-, rt 0.58 min, LC-MS Method b.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 667463-64-1.

Electric Literature of 18711-15-4,Some common heterocyclic compound, 18711-15-4, name is 4,6-Dichloroisatin, molecular formula is C8H3Cl2NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: A reaction flask with high vacuum valve was charged with 2-amino-N?-arylbenzohydrazides (1.0 mmol), 4-halogenated isatins (1.0 mmol), CuI (10 mg, 0.05 mmol), and Cs2CO3 (650 mg, 2.0 mmol). After being degassed by three freeze-thaw pump cycles, THF (10.0 mL) was injected into the mixture. And then, the reaction mixture was stirred at reflux for 10-16 h before reaching completion, which was monitored by TLC. The solvent was recovered by distillation under reduced pressure, and the residue was purified by chromatography over silica gel to give 3 using ethyl acetate and petroleum ether (1:2) as an eluent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4,6-Dichloroisatin, its application will become more common.

Application of 550-44-7, The chemical industry reduces the impact on the environment during synthesis 550-44-7, name is 2-Methylisoindoline-1,3-dione, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of magnesium (1.0 M in THF, 22 mL, 23.8 mmmol) was added 4-bromo-1-butene (2.2mL, 22 mmol) under a nitrogen atmosphere. After stirring the mixture for 30 min, the resultingsolution was added to the solution of N-methylphthalimide (1.42 g, 6.38 mmol) in THF (34 mL) at-20 C and stirred for additional 1 hour at the same temperature. The reaction was quenched byaddition of saturated aqueous NH4Cl (20 mL), and the resulting solution was extracted with EtOAc(30 mL). The organic extracts were washed with brine (20 mL), dried over Na2SO4, filtered, andconcentrated in vacuo to give a crude material (1.61 g). To a solution of the crude material (1.61 g) in dichloromethane (68 mL) was added triethylsilane (4.3mL, 27 mmmol) and boron trifluoride diethyl ether complex (3.4 mL, 27 mmol) under a nitrogenatmosphere at -20 C. The mixture was allowed to warm to 0 C and stirred for 30 min. The reactionwas quenched by addition of saturated aqueous NaHCO3 (50 mL). The resulting solution wasextracted with EtOAc (60 mL). The organic extracts were washed with brine (50 mL), dried overNa2SO4, filtered, and concentrated in vacuo to give a crude material. This material was purified bycolumn chromatography (silica gel, hexane/EtOAc = 3/1 to 1/1) to give 3a (1.17 g, 5.81 mmol, 85%for 2 steps) as a pale yellow oil.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Methylisoindoline-1,3-dione, other downstream synthetic routes, hurry up and to see.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 16800-68-3, name is 1-Acetylindolin-3-one belongs to indolines-derivatives compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C10H9NO2

e) 2-(1-Acetyl-1H-indol-3-yl)-5,5-dimethylcyclohexane-1,3-dione 1-Acetyl-1,2-dihydroindol-3-one of Example 1d (131.3 g, 0.75 mol) and 5,5-dimethyl-cyclohexane-1,3-dione (105 g, 0.75 mol) were added to a mixture of acetic acid (700 mL) and triethylamine (105 mL, 0.75 mol) at room temperature under stirring. The reaction mixture was refluxed for 6 h. About 1/3 volume of solvents was removed in vacuum, and the mixture was cooled and diluted with water (50 mL). The precipitate was filtered off, washed with ethanol-water, 1:1 and dried to afford 169.4 g (76%) of colorless crystals; m.p. 225-227 C.

The synthetic route of 16800-68-3 has been constantly updated, and we look forward to future research findings.

Application of 17564-64-6, A common heterocyclic compound, 17564-64-6, name is 2-(Chloromethyl)isoindoline-1,3-dione, molecular formula is C9H6ClNO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: Conditions A: aqueous 37% hydrochloric acid (0.17 mL, 2 mmol) was added to a solution of 1 (258 mg, 1.0 mmol) in 8 mL of degassed ethanol. The mixture was heated at 95 C under Argon atmosphere until the selenocarbonate 1 disappeared (2,5-3 h). After cooling to room temperature sodium bicarbonate (0.34 g, 4 mmol) and alkylhalide (1.5 mmol, see Table 3) were added and the resulting mixture was stirred until the end of the reaction (TLC analysis). After the addition of water (10 mL) the mixture was extracted three times with 10 mL of EtOAc. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated in vacuo. The residue was purified on a silica gel column with a mixture of petroleum ether and ethyl ether as eluant to give the corresponding selenide 5. Conditions B: trifluoroacetic acid (0.15 mL, 2 mmol) was added to a solution of 1 (258 mg, 1.0 mmol) in 8 mL of degassed DMF. The mixture was heated at 95 C under Argon atmosphere until the selenocarbonate 1 disappeared (2,5-3 h). After cooling to room temperature sodium acetate (0.33 g, 4 mmol) and alkyl or aryl halide (1.5 mmol, see Table 3) were added and the resulting mixture was stirred until the end of the reaction (TLC analysis). After the addition of water (10 mL) the mixture was extracted three times with 10 mL of EtOAc. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated in vacuo. The corresponding selenide 5 was isolated after column chromatographyon SiO2 utilizing a mixture of diethyl ether and petroleum ether as eluant. Characterisation data for selenides 5b-5c [26], 5d, [27] 5e, [28] 5f [29], 5g [30], 5h [31], and 5i [32] matched the ones previously reported in literature for these compounds.

The synthetic route of 17564-64-6 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 17564-64-6,Some common heterocyclic compound, 17564-64-6, name is 2-(Chloromethyl)isoindoline-1,3-dione, molecular formula is C9H6ClNO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

tert-Butyl 3-bromo-4-oxo-piperidine-1-carboxylate (2 g, 7.2 mmol) was suspended in THF (2 mL) and cooled in an ice bath before addition of dimethylamine (16 mL of 2 M, 32 mmol). Upon complete addition, the ice bath was removed and the mixture was stirred at ambient temperature for 16 hours. The mixture was partitioned between saturated aqueous sodium bicarbonate solution and EtOAc. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo. The residue was dissolved in THF (28 mL) under N2. The solution was cooled to -78 C and LiHMDS (10 mL of 1 M, 10 mmol) was added dropwise. After 40 minutes, 2- (chloromethyl)isoindoline-1,3-dione (2.32 g, 11.8 mmol) was added in portions over 5 minutes. The solution was stirred for 1 hour then left to warm up to 0 C before being quenched by addition of saturated aqueous NH4Cl solution. The mixture was partitioned between saturated aqueous sodium bicarbonate solution and EtOAc. The organic layer was separated, dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (silica, 0-10% MeOH/DCM gradient elution) to give tert-butyl 3-(dimethylamino)-5-[(1,3-dioxoisoindolin-2- yl)methyl]-4-oxo-piperidine-1-carboxylate (1.58 g, 50%); MS m/z: 402 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(Chloromethyl)isoindoline-1,3-dione, its application will become more common.

Related Products of 104618-32-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 104618-32-8 as follows.

A solution of N-(4-oxocyclohexyl)phthalimide (14, 5.00 g, 21 mmol, 1 eq.) and 4-methoxyphenylhydrazine hydrochloride (3.59 g, 21 mmol, 1 eq.) in dry ethanol (100 mL) was heated at reflux for 2.5 h. After cooling down to room temperature, the precipitate was filtrated off and washed with ethanol 96% (3 * 10 mL). The solid was dried under reduced pressure and freeze-dried overnight. Rf = 0.66 (cyclohexane/ethyl acetate/dimethylethylamine 5:5:0.2). Colorless solid, mp 222-223 C, yield 6.88 g (97%). Purity (HPLC): 84.1% (tR = 22.2 min). C21H18N2O3 (346.4 g/mol). Exact mass (APCI): m/z = 347.1389 (calcd. 347.1390 for C21H19N2O3 [M + H+]). 1H NMR (400 MHz, DMSO-D6): delta (ppm) = 2.03-2.11 (m, 1H, 2-H), 2.67 (tt, J = 12.3/6.4 Hz, 1H, 2-H), 2.80-2.98 (m, 3H, 1-CH2, 4-H), 3.20-3.28 (m, 1H, 4-H), 3.71 (s, 3H, OCH3), 4.43-4.52 (m, 1H, 3-H), 6.65 (dd, J = 8.7/2.4 Hz, 1H, 7-H), 6.82 (d, J = 2.4 Hz, 1H, 5-H), 7.15 (d, J = 8.7 Hz, 1H, 8-H), 7.84-7.91 (m, 4H, 4-Hphth, 5-Hphth, 6-Hphth, 7-Hphth), 10.61 (s, 1H, NH). 13C NMR (101 MHz, DMSO-D6): delta (ppm) = 22.6 (1C, C-1), 24.7 (1C, C-4), 26.5 (1C, C-2), 47.8 (1C, C-3), 55.3 (1C, OCH3), 99.7 (1C, C-5), 106.3 (1C, C-4a), 109.9 (1C, C-7), 111.2 (1C, C-8), 123.0 (2C, C-4phth, C-7phth), 127.2 (1C, C-4b), 131.3 (1C, C-8a), 131.5 (2C, C-3aphth, C-7aphth), 134.2 (1C, C-9a), 134.4 (2C, C-5phth, C-6phth), 153.0 (1C, C-6), 167.9 (2C, C=O). FTIR (neat): ? (cm-1) = 3425 (w, N-H), 3379 (w, C-H, arom), 2924 (w, C-H, aliph), 1697 (s, C=O), 1597 (w, C-C, arom).

According to the analysis of related databases, 104618-32-8, the application of this compound in the production field has become more and more popular.

Reference of 611-09-6, A common heterocyclic compound, 611-09-6, name is 5-Nitroindoline-2,3-dione, molecular formula is C8H4N2O4, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: A mixture of isatin derivatives (1a-1d, 1 mmol) oracenaphthoquinone (5, 1 mmol), methylene nitriles (2a,2b, 1 mmol), 1,3-dicarbonyl (3, 1 mmol), and 5 mg IG in3 cm3 H2O was stirred at 60 C for the mentioned timeshown in tables. Rapid conversion of reagents can beclearly confirmed by reaction color change. The progress ofthe reaction was monitored by TLC using EtOAc/n-hexane(1:3) as an eluent. Upon completion, the reaction mixturewas allowed to cool to room temperature and the precipitatewas obtained from the reaction mixture by filtration.The product 4a was dissolved in DMSO and the catalystwas separated by simple filtration. Pure products wereafforded by evaporation of the solvent under reduced pressure.

The synthetic route of 611-09-6 has been constantly updated, and we look forward to future research findings.