HRID130613

反应详情

EQUATION

反应方程式

HRID 130613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium borohydride (170 mg, 4.50 mmol) was added to and dissolved in N,N-dimethylacetamide (1.5 mL) at room temperature, followed by addition of an N,N-dimethylacetamide solution (1.0 mL) of ethyl 1-chloro-2-fluoro-cyclopropane-1-carboxylate (hereinafter the compound will be referred to as “compound (1b)”) (cis/trans=95/5) (500 mg, 3.00 mmol). Cobalt chloride hexahydrate (3.6 mg, 0.015 mmol) was added to the resultant solution at the same temperature. After completion of addition, the resultant mixture was stirred at 40° C. for one hour. After completion of reaction, the whole reaction mixture was diluted with an HPLC mobile phase to 50 mL, to thereby yield a solution containing 381.3 mg (yield: 96%) of the title compound. Yield was determined by means of high performance liquid chromatography (HPLC) (the same shall apply hereinafter).

WORKUP

后处理

  1. additionAfter completion of addition
  2. customAfter completion of reaction
  3. customthe whole reaction mixture
  4. additionwas diluted with an HPLC mobile phase to 50 mL
  5. customto thereby yield a solution