HRID9802

反应详情

EQUATION

反应方程式

HRID 9802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a stirred solution of 6-cyclobutylidene-hexanoic acid methyl ester (0.60 g, 3.3 mmol) in toluene (30 mL) was added DIBAL-H (8.2 mL, 1 M solution in hexane, 8.2 mmol) dropwise at 0° C. under N2. After stirring at 0° C. for 30 min, the reaction was quenched by MeOH (3 mL). Saturated aqueous sodium potassium tartrate (20 mL) was added to the reaction mixture. After stirrng for 1 h, the organic layer was separated and the aqueous phase was extracted with ether. The combined organic layers were washed with water and brine and dried. Evaporation of the solvent gave 6-cyclobutylidene-hexan-1-ol as a colorless oil, which was used in the next step without further purification.

WORKUP

后处理

  1. customthe reaction was quenched by MeOH (3 mL)
  2. additionSaturated aqueous sodium potassium tartrate (20 mL) was added to the reaction mixture
  3. waitAfter stirrng for 1 h
  4. customthe organic layer was separated
  5. extractionthe aqueous phase was extracted with ether
  6. washThe combined organic layers were washed with water and brine
  7. customdried
  8. customEvaporation of the solvent