Carbon Dioxide → Phenylbenzylglyoxal

HRID 442413

반응식

HRID 442413 반응식
[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

참가 물질

6

반응물 4

HCID 280Carbon Dioxide2회HCID 962WaterHCID 92219Chalcone epoxideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 11096234Phenylbenzylglyoxal수율 65%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-972728a6b5bd4f92b2f0a83fcfe80e4f
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04045487

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