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 3339-73-9 as follows. Formula: C11H9NO4
Oxalyl chloride (5.8 ml; 66.7 mmol) is added to Pht-beta-Ala-OH (9.96 g; 44.5 mmol) dissolved in dichloromethane (120 ml) and 3 drops of dimethylformamide (DMF). The mixture is stirred for 3 hours at ambient temperature. After elimination of the solvent, the white solid is taken up in a 1:1 mixture of anhydrous tetrahydrofuran and acetonitrile (200 ml) then 49 ml of a 2 M solution of (trimethylsilyl) diazomethane in hexane (97.9 mmol) are added dropwise at 0 C. The solvents are eliminated after one night of stirring at 0 C. The pale yellow solid is then dissolved in dichloromethane (60 ml) and 12 ml of aqueous hydrobromic acid (48%) is added dropwise at 0 C. The mixture is stirred until the temperature reaches 15 C. and 50 ml of a saturated solution of sodium bicarbonate is added. The organic phase is washed with salt water then dried over sodium sulphate. Crystallization from diethyl ether allows a white solid to be obtained (11.39 g; yield=86%). [00199] NMR 1H (DMSO D6, 100 MHz, delta): 7.83 (s, 4H); 4.36 (s, 2H, CH2Br); 3.8 (t, 2H, J=7.1 Hz, NCH2); 2.98 (t, 2H, J=6.9 Hz, CH2CO).
According to the analysis of related databases, 3339-73-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Societe de Conseils de Recherches et d’Applications Scientifiques (S.C.R.A.S.); US6727269; (2004); B1;,
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Indoline | C8H9N – PubChem