HRID1513539

反应详情

EQUATION

反应方程式

HRID 1513539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 214.9 g portion of the above-mentioned crude 6-chloro-3-oxo-hexanoic acid methyl ester (1), Ru2Cl4-[(S)-Segphos]2(NEt)3 (60.7 mg, 0.0725×10−3 mol) and methanol (130 ml) were put into a 500 ml capacity autoclave and stirred with hydrogen (3 MPa) at 65 to 70° C. for 6 hours. After completion of the reaction, the solvent was evaporated under a reduced pressure using an evaporator, and then the residue was distilled under a reduced pressure (75 to 85° C./0.1 ton) to obtain 6-chloro-3-hydroxy-hexanoic acid methyl ester (2); 178.2 g {GC purity; 80.1%, pure amount; 142.7 g (0.790 mol, yield 44%/4-chlorobutanoic acid chloride)}.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated under a reduced pressure
  3. customan evaporator
  4. distillationthe residue was distilled under a reduced pressure (75 to 85° C./0.1 ton)