HRID371159

反应详情

EQUATION

反应方程式

HRID 371159 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A mixture of 778 mg (1.90 mmole) of cis-2-[2-benzyloxy-4-(1,1-dimethylheptyl)phenyl]-4-piperidinol, 160 microliters (1.84 mmole) of 1-bromo-2-propene and 300 mg (2.17 mmole) of potassium carbonate in 10 ml ethanol is stirred at 25° C. for 20.5 hours. An additional 4 microliters of 1-bromo-2-propene is added to the reaction and stirring continued for 7 hours. The reaction mixture is then added to 50 ml saturated sodium chloride and extracted with 250 ml ethyl ether. The ether extract is dried over magnesium sulfate and the solvent is evaporated. The resulting oil is purified via column chromatography on 28 g of silica gel eluted in 7 ml fractions with 1:3 methanol/ethyl ether to yield (fractions 10-35) 518 mg (61%) of the title compound as an oil.

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued for 7 hours
  3. extractionextracted with 250 ml ethyl ether
  4. extractionThe ether extract
  5. dry with materialis dried over magnesium sulfate
  6. customthe solvent is evaporated
  7. customThe resulting oil is purified via column chromatography on 28 g of silica gel
  8. washeluted in 7 ml fractions with 1:3 methanol/ethyl ether