HRID1534554

反应详情

EQUATION

反应方程式

HRID 1534554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 365 mg of (racemic)-3-methoxypyrrolidine, 530 mg of N-propargyl-2-pyrrolidinone, 180 mg of paraformaldehyde, 0.6 ml of acetic acid, 20 ml of dioxane and 10 mg of cuprous chloride was stirred at reflux under argon for 1 hour. The reaction was cooled and treated with a mixture of 3 ml of 5N sodium hydroxide and 2 ml of water. The mixture was extracted twice with dichloromethane. The extracts were combined, dried, filtered and concentrated in vacuo to an oil. The oil was purified by chromatography (alumina), giving 520 mg of the desired product as a yellow oil.

WORKUP

后处理

  1. temperatureat reflux under argon for 1 hour
  2. temperatureThe reaction was cooled
  3. extractionThe mixture was extracted twice with dichloromethane
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo to an oil
  7. customThe oil was purified by chromatography (alumina)