3-甲基-2-丁酮 → Tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate

HRID 972709笔记

反应方程式

HRID 972709 反应方程式
[CH:1]([C:4]([CH3:6])=[O:5])([CH3:3])[CH3:2].Cl[CH:8]([Cl:16])[C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10]>O1CCCC1>[Cl:16][C:8]1([O:5][C:4]1([CH:1]([CH3:3])[CH3:2])[CH3:6])[C:9]([O:11][C:12]([CH3:13])([CH3:14])[CH3:15])=[O:10]

参与物

4

反应物 2

HCID 112513-甲基-2-丁酮HCID 30164832,2-二氯乙酸叔丁酯

产物 1

HCID 21443884Tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate收率 98.2%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂

实验过程

A solution of 122 g of potassium tert.-butylate in 720 ml of tetrahydrofuran was added at -20° C. with stirring under an inert atmosphere to a mixture of 95 g of methyl isopropyl ketone and 185 g of tert.butyl dichloroacetate and after returning the temperature to room temperature, the mixture was stirred for 2 hours. The mixture was poured into ice water and the mixture was stirred and the organic phase was separated. The organic phase was washed with aqueous sodium chloride solution, dried over magnesium sulfate, passed through vegetable charcoal and concentrated to dryness to obtain 230.4 g of tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate.

后处理

  1. customto room temperature
  2. stirringthe mixture was stirred
  3. customthe organic phase was separated
  4. washThe organic phase was washed with aqueous sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated to dryness

来源与证据

ORD记录
ord-d9affb2b65f3455eaf12a6d03e58495f
来源数据集
uspto-grants-1977_10
专利号
US04053597

反应笔记

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