HRID2078489

反应详情

EQUATION

反应方程式

HRID 2078489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

From 4041 g of the resultant solution, 20.1 g of that was used, and the subsequent cis body/trans body separation operation was carried out. Into 20.1 g of this solution, a 20% sodium hydroxide aqueous solution was dropped, to adjust pH of the solution to 3. An extraction operation was repeated three times from this solution with 7.8 kg of toluene, and the resultant organic layers were combined. Then, toluene was distilled off, then, 1.49 g of a solution containing 1.17 g of 6,6-dimethyl-3-oxabicyclo[3.1.0]hexan-2-one (9.27 mmol, yield based on ethyl cis-3-acetoxymethyl-2,2-dimethylcyclopropanecarboxylate: 97.2%, (1R, 5S)-body had an optical purity of 92.8% ee) was obtained. In this toluene solution, 0.057 g (0.39 mmol) of trans-3-hydroxymethyl-2, 2-dimethylcyclopropanecarboxylic acid was present.

WORKUP

后处理

  1. customthe subsequent cis body/trans body separation operation
  2. additionInto 20.1 g of this solution, a 20% sodium hydroxide aqueous solution was dropped
  3. distillationThen, toluene was distilled off
  4. addition1.49 g of a solution containing 1.17 g of 6,6-dimethyl-3-oxabicyclo[3.1.0]hexan-2-one (9.27 mmol
  5. customyield
  6. customwas obtained