HRID273327

反应详情

EQUATION

反应方程式

HRID 273327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Methoxy-2-methylpyridine (0.123 g, 1 mmol) and bromoacetone (0.16 mL, 1 mmol) were heated at 95° C. under N2 for 2 h. 1,8-Diazabicyclo-[5.4.0]-undec-7-ene (0.34 mL, 2.2 mmol) in benzene (10 mL) was added. The mixture was then refluxed under N2 for 1 h, poured into ice water, and then extracted with EtOAc. The combined organic layers were washed with water and dried. After the solvent was removed in vacuo, the residue was purified on a silica gel column eluting with EtOAc:Hexane (1:9) and EtOAc to give 7-methoxy-2-methylindolizine (0.050 g, 31%).

WORKUP

后处理

  1. temperatureThe mixture was then refluxed under N2 for 1 h
  2. extractionextracted with EtOAc
  3. washThe combined organic layers were washed with water
  4. customdried
  5. customAfter the solvent was removed in vacuo
  6. customthe residue was purified on a silica gel column
  7. washeluting with EtOAc:Hexane (1:9) and EtOAc