HRID1180558
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of methyl 2-[(2-acetylamino-benzyl)-(4-methoxybenzenesulfonyl)amino]acrylate (8.40 g, 20.07 mmol) in anhydrous methanol (5 ml) was added anhydrous sodium bicarbonate (2.19 g, 26.09 mmol) and the mixture was stirred at room temperature overnight. Anhydrous sodium bicarbonate (2.2 g) was added and the mixture was stirred for 18 hours, heated to 50° C. for three hours and the solvent removed in vacuo. The residue was dissolved in water and ethyl acetate. The organic layer was separated, washed with saturated sodium chloride and dried with anhydrous sodium sulfate. The solvent was removed in vacuo and the residue dried in vacuo to give 6.64 g of white crystals, m.p. 150-155° C.
WORKUP
后处理
- stirringthe mixture was stirred for 18 hours
- temperatureheated to 50° C. for three hours
- customthe solvent removed in vacuo
- dissolutionThe residue was dissolved in water
- customThe organic layer was separated
- washwashed with saturated sodium chloride
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was removed in vacuo
- customthe residue dried in vacuo