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碳酸锂 → Tert.-butyl 3-isopropyl-2-oxo-3-butenoate

HRID 972710
笔记
打印预览

反应方程式

HRID 972710 反应方程式
[Br-].[Li+].Cl[C:4]1([O:17][C:12]1([CH:14]([CH3:16])[CH3:15])[CH3:13])[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6].C(=O)([O-])[O-].[Li+].[Li+]>O>[CH:14]([C:12](=[CH2:13])[C:4](=[O:17])[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6])([CH3:16])[CH3:15]
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 11125碳酸锂HCID 82050溴化锂HCID 21443884Tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate

产物 1

HCID 21405096Tert.-butyl 3-isopropyl-2-oxo-3-butenoate收率 85.2%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
5 °C

实验过程

118 g of anhydrous lithium bromide were added under an inert atmosphere to a mixture of 117.5 g of tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate and 18.5 g of lithium carbonate in 1.15 liters of hexamethylphosphonotriamide cooled to 5° C. and after the temperature was returned to room temperature, the mixture was stirred under a nitrogen atmosphere for 48 hours. 500 ml of distilled water were added thereto and the mixture was poured into an ampoule containing a mixture of water-petroleum ether (9-1). The mixture was decanted and the aqueous phase was extracted with petroleum ether. The combined ether phases were washed with water, dried over magnesium sulfate and the petroleum ether was evaporated under reduced pressure to obtain 84.6 g of tert.-butyl 3-isopropyl-2-oxo-3-butenoate.

后处理

  1. customwas returned to room temperature
  2. additionthe mixture was poured into an ampoule
  3. additioncontaining
  4. customThe mixture was decanted
  5. extractionthe aqueous phase was extracted with petroleum ether
  6. washThe combined ether phases were washed with water
  7. dry with materialdried over magnesium sulfate
  8. customthe petroleum ether was evaporated under reduced pressure

来源与证据

ORD记录
ord-d4c54c2751184d6b91375a4bec456f4e
来源数据集
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US04053597

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记