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 60434-13-1 as follows. HPLC of Formula: C9H6ClNO2
General procedure: To a stirred solution of isatin 6 (20 mmol) in dry DMF (30 mL), K2CO3 (30 mmol) wasadded and stirred for 10 min. 7 (24 mmol) was added dropwise to the reaction mixture. Thereaction mixture was then stirred at room temperature overnight. Ice water was added and theprecipitate produced which was collected by filtration. Orange solid 8 was obtained afterdried by vacuum. Solid 8 was then dissolved in NH2NH2H2O (20 mL) and the reaction mixture washeated to 130 oC. After 3 h, the reaction was cooled and diluted with EtOAc. The aqueouslayer was extracted with EtOAc. The combined organic layer was washed with saturatedaqueous NaHCO3, brine, dried over anhydrous Na2SO4 and concentrated under reducedpressure. The residue 9 was used directly without purified. To a suspension of NaH in THF, N-substitued oxoindole 9 was added by portion in 0 oC.after stirred for 10 minutes, correspond isocyanate was added by potions. The mixture wascontinue stirred overnight. It was quenched by 1M HCl to adjust the PH to 2~5 and thendiluted with EtOAc. The water layer was extracted with EtOAc. The combined organic layerwas washed with water, brine, dried over anhydrous Na2SO4 and concentrated under reducedpressure. The residue was purified by column chromatography on silica gel. (PE/EA = 5/1) togive compound 1a-1r as a white solid.
According to the analysis of related databases, 60434-13-1, the application of this compound in the production field has become more and more popular.
Reference:
Article; Chen, Hui; Liu, Hui; Zhao, Si-Han; Cheng, Shao-Bing; Xu, Xiao-Ying; Yuan, Wei-Cheng; Zhang, Xiao-Mei; Synlett; vol. 30; 9; (2019); p. 1067 – 1072;,
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