HRID1261916

反应详情

EQUATION

反应方程式

HRID 1261916 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2 M of Sodium hypochlorite in Water (750 mL) (10-14% solution) was added dropwise to a solution of 1H-Pyrrole-2-carboxylic acid ethyl ester (50.0 g, 359 mmol), 2-Methoxy-2-methylpropane (1000 mL), Aliquot 336 (12 g, 31 mmol), 7 M of Sodium hydroxide in Water (1030 mL), 8 M of Ammonium hydroxide in Water (330 mL) and Ammonium chloride (120 g, 2200 mmol). The reaction was immediately worked up upon complete addition of sodium hypochlorite. The organic layer was separated and was washed with saturated sodium thiosulfate (3×500 mL). Organic extracts (3×500 mL) were dried over magnesium sulfate, filtered and reduced to afford 53.0 grams 1-Amino-1H-pyrrole-2-carboxylic acid ethyl ester as a brown oil without further purification.

WORKUP

后处理

  1. customThe organic layer was separated
  2. washwas washed with saturated sodium thiosulfate (3×500 mL)
  3. dry with materialwere dried over magnesium sulfate
  4. filtrationfiltered