HRID1732431

反应详情

EQUATION

反应方程式

HRID 1732431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 1.38 g quantity of potassium carbonate and 308 mg of potassium iodide are placed into a reactor. Acetone (30 ml) and a solution of 450 mg of methyl 4-tert-butoxycarbonyl-3-dimethoxymethyl-5-oxohexanoate in 10 ml of acetone are further placed into the reactor. Subsequently 270 mg of pentynyl bromide is added to the mixture. The resulting mixture is stirred at room temperature for one hour and thereafter refluxed at 70° C. for 13 hours. On completion of the reaction, the mixture is cooled to room temperature, and the solids are separated off. The product is concentrated in a vacuum, and the residue purified by a silica gel column, giving methyl 4-acetyl-4-tert-butoxycarbonyl-3-dimethoxymethyl-6-nonynoate (compound (8), R1 =t-Bu, R2 =R3 =CH3) in a yield of 91%.

WORKUP

后处理

  1. temperaturerefluxed at 70° C. for 13 hours
  2. customOn completion of the reaction
  3. temperaturethe mixture is cooled to room temperature
  4. customthe solids are separated off
  5. concentrationThe product is concentrated in a vacuum
  6. customthe residue purified by a silica gel column