Carbon Dioxide → Phenylbenzylglyoxal

HRID 918082

反応式

HRID 918082 の反応式
[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>CO.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

参加物

7

反応物 4

HCID 280Carbon Dioxide2 回HCID 962WaterHCID 92219Chalcone epoxideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 11096234Phenylbenzylglyoxal収率 65%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

To a boiling solution of 30 g 1,3-diphenyl-2,3-epoxy-1-propanone in 500 ml methanol 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.

後処理

  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

出典と根拠

ORDレコード
ord-eab7f811fe8246d29aa555e53bba1784
出典データセット
uspto-grants-1976_07
特許番号
US03969373

関連ノート

読み込み中…