HRID385785

反应详情

EQUATION

反应方程式

HRID 385785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

A solution of 1-(6-bromopyridin-2-yl)methanamine hydrochloride (500 mg, 2.24 mmol) in toluene (10 ml) was charged with triethylamine (0.31 ml, 2.24 mmol). The reaction was stirred for 5 minutes after which cyclopentane-1,3-dione (330 mg, 3.36 mmol) and p-toluenesulfonic acid monohydrate (43 mg, 0.022 mmol) were added. The reaction mixture was heated to reflux at 95° C. for 45 minutes. The reaction mixture was cooled to ambient temperature and diluted with ethyl acetate (15 ml), 2N sodium hydroxide (10 ml) and brine (10 ml). The layers were separated and the organic layer was then dried over sodium sulfate, filtered and concentrated to yield the title compound.

WORKUP

后处理

  1. additionwere added
  2. temperatureThe reaction mixture was heated
  3. temperatureThe reaction mixture was cooled to ambient temperature
  4. customThe layers were separated
  5. dry with materialthe organic layer was then dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated