碳酸钾 → HCID 20309567，化合物

HRID 972795笔记

反应方程式

HRID 972795 反应方程式
[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([OH:19])=[C:9]([CH:18]=1)[C:10]([CH2:12][CH2:13][C:14]([O:16][CH3:17])=[O:15])=[O:11])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[CH2:26]([CH:28]1[O:30][CH2:29]1)Br>CC(CC)=O>[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([O:19][CH2:26][CH:28]2[O:30][CH2:29]2)=[C:9]([CH:18]=1)[C:10]([CH2:12][CH2:13][C:14]([O:16][CH3:17])=[O:15])=[O:11])(=[O:3])[CH3:2]

参与物

5

反应物 3

HCID 11430碳酸钾HCID 18430环氧溴丙烷HCID 20309539HCID 20309539，化合物

产物 1

HCID 20309567HCID 20309567，化合物收率 57.8%

试剂、催化剂与溶剂 1

HCID 6569Methyl Ethyl Ketone溶剂

实验过程

Methyl 3-(5-acetamido-2-hydroxybenzoyl)propionate (0.75 g, 0.0028 mole), anhydrous potassium carbonate (0.39 g, 0.0028 mole), epibromohydrin (0.78 g, 0.00565 mole) and dry ethyl methyl ketone (20 ml) were stirred and heated under reflux for 16 hours. The cooled mixture was filtered and evaporated under reduced pressure to an oil which was purified by elution from a silica column with chloroformmethanol to give methyl 3-[5-acetamido-2-(2,3-epoxypropoxy)benzoyl]propionate (0.52 g, 57%, m.p. 84°-87°).

后处理

  1. temperatureheated
  2. temperatureunder reflux for 16 hours
  3. filtrationThe cooled mixture was filtered
  4. customevaporated under reduced pressure to an oil which
  5. customwas purified by elution from a silica column with chloroformmethanol

来源与证据

ORD记录
ord-5f1724c00f9f470f82941ac178734acc
来源数据集
uspto-grants-1977_10
专利号
US04053601

反应笔记

加载中…