HRID1180558

反应详情

EQUATION

反应方程式

HRID 1180558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringthe mixture was stirred for 18 hours
  2. temperatureheated to 50° C. for three hours
  3. customthe solvent removed in vacuo
  4. dissolutionThe residue was dissolved in water
  5. customThe organic layer was separated
  6. washwashed with saturated sodium chloride
  7. dry with materialdried with anhydrous sodium sulfate
  8. customThe solvent was removed in vacuo
  9. customthe residue dried in vacuo