二氧化碳 → Diphenylethanone Impurity 2

HRID 442413

反应方程式

HRID 442413 反应方程式
[C:1]1([C:7](=[O:17])[CH:8]2[O:10][CH:9]2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CC(C)([O-])C.[K+].O.C(=O)=O>C(O)C>[C:1]1([C:7](=[O:17])[C:8](=[O:10])[CH2:9][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参与物

6

反应物 4

HCID 280二氧化碳2 次HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 92219查耳酮ALPHA环氧化物HCID 23665647叔丁醇钾

产物 1

HCID 11096234Diphenylethanone Impurity 2收率 65%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂2 次

实验过程

To a boiling solution of 30 g 1,3-diphenyl-2,3-epoxy-1-propanone in 500 ml ethanol was rapidly added a hot solution of 30 g potassium t-butoxide in 500 ml ethanol. The mixture was kept boiling on a steambath for 2 minutes. It was then diluted with 3 l. water. The aqueous solution was saturated with carbon dioxide by the addition of small pieces of dry ice. The resulting emulsion was extracted with ether. The ether extracts were diluted with benzene, dried over sodium sulfate and evaporated under reduced pressure. The remaining dark oil was distilled in high vacuum to afford 19.5 g 1,3-diphenyl-1,2-propanedione; b.p. 136°-138°/0.1 mm.

后处理

  1. additionIt was then diluted with 3 l
  2. extractionThe resulting emulsion was extracted with ether
  3. additionThe ether extracts were diluted with benzene
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure
  6. distillationThe remaining dark oil was distilled in high vacuum

来源与证据

ORD记录
ord-972728a6b5bd4f92b2f0a83fcfe80e4f
来源数据集
uspto-grants-1977_08
专利号
US04045487

关联笔记

加载中…