HRID1513539
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter completion of the reaction
- customthe solvent was evaporated under a reduced pressure
- customan evaporator
- distillationthe residue was distilled under a reduced pressure (75 to 85° C./0.1 ton)