HRID239100

反应详情

EQUATION

反应方程式

HRID 239100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.7 mL 33% HBr in acetic acid and 11.4 g bromine in 30 mL acetic acid were added slowly to a stirred solution of 10 g piperidin-4-one in 60 mL acetic acid at RT. The reaction mixture was stirred for additional 45 min at ambient temperature and the acetic acid was completely removed under reduced pressure. The residue was dissolved in 200 mL acetone and refluxed for 1 h, cooled, filtered and washed with acetone and dried to give 15.2 g of the desired product, (M+H)+: 180.

WORKUP

后处理

  1. customthe acetic acid was completely removed under reduced pressure
  2. dissolutionThe residue was dissolved in 200 mL acetone
  3. temperaturerefluxed for 1 h
  4. temperaturecooled
  5. filtrationfiltered
  6. washwashed with acetone
  7. customdried