反应详情

To a stirring solution of Methyl 3-[4-(2-acetylhydrazinecarbonyl)phenoxy]-5-(benzyloxy)benzoate (32 g) (Intermediate 9) in dry toluene was added thionyl chloride (10.5 g) drop wise at room temperature under nitrogen atmosphere. The reaction was refluxed and monitored by TLC. After completion of the reaction, reaction mixture was diluted with water and extracted with EtOAc. All organic layers were combined and washed with saturated sodium bicarbonate solution, water, and brine, dried over anhydrous sodium sulphate, filtered and concentrated under vacuum to get crude pale yellow solid (30 g). The crude compound was purified by solvent trituration.

1. temperatureThe reaction was refluxed
2. customAfter completion of the reaction, reaction mixture
3. extractionextracted with EtOAc
4. washwashed with saturated sodium bicarbonate solution, water, and brine
5. dry with materialdried over anhydrous sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated under vacuum