HRID249307

反应详情

EQUATION

反应方程式

HRID 249307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Acetyl-3-bromo-4-piperidone hydrobromide (5.0 g, 16.6 mmol) in acetone (160 ml) was heated to 60° and treated with triethylamine (2.31 ml, 33.1 mmol) and thioacetamide (1.24 g, 16.6 mmol). The reaction mixture was heated to reflux for 24 hours, then cooled and filtered, to provide a yellow solid which was purified by column chromatography (eluant: 89:10:1 chloroform: methanol: concentrated aqueous ammonium hydroxide). The title product was obtained as a yellow oil (995 mg, 5.1 mmol, 31% yield).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. customto provide a yellow solid which
  6. customwas purified by column chromatography (eluant: 89:10:1 chloroform: methanol: concentrated aqueous ammonium hydroxide)