HRID1054213

反应详情

EQUATION

反应方程式

HRID 1054213 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

To a stirring solution of ethyl hydrogen malonate (0.6 g, 4.54 mmol) and ethyl 2-(benzyloxyamino)benzoate (1.12 g, 4.13 mmol) in acetonitrile (10 mL) was added pyridine (1.3 g, 16.51 mmol) and reaction mixture was cooled to 0-10° C. To this was added POCl3 (0.423 mL, 4.54 mmol), at 0-10° C. in 15-30 min. and stirring continued for 1 h. Reaction mixture was diluted with DCM and washed with water. Organic layer was separated and distilled out to get crude product which was column purified using 15% EtOAC in hexane to get titled compound in 79% yield.

WORKUP

后处理

  1. waitcontinued for 1 h
  2. customReaction mixture
  3. washwashed with water
  4. customOrganic layer was separated
  5. distillationdistilled out
  6. customto get crude product which
  7. custompurified