Potassium Carbonate → [3-(Dimethoxymethyl)-4-nitrophenyl]phenylmethanone

HRID 2247888노트

반응식

HRID 2247888 반응식
[CH3:1][O:2][CH:3]([O:22][CH3:23])[C:4]1[CH:5]=[C:6]([CH:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)C#N)[CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11].C(=O)([O-])[O-:25].[K+].[K+]>CN(C)C(=O)C>[CH3:1][O:2][CH:3]([O:22][CH3:23])[C:4]1[CH:5]=[C:6]([C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[O:25])[CH:7]=[CH:8][C:9]=1[N+:10]([O-:12])=[O:11]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 198160313-(Dimethoxymethyl)-4-nitro-alpha-phenylbenzeneacetonitrile

생성물 1

HCID 19816024[3-(Dimethoxymethyl)-4-nitrophenyl]phenylmethanone수율 67.3%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A mixture of 26.7 parts of intermediate 9, namely 3-(dimethoxymethyl)-4-nitro-α-phenylbenzeneacetonitrile, 12.3 parts of potassium carbonate and 360 parts of N,N-dimethylacetamide was stirred at room temperature while bubbling air through it. The reaction mixture was poured into water and the whole was extracted with dichloromethane. The extract was dried, filtered and evaporated and the residue was purified by column chromatography (silica gel; CHCl3 /hexane 80:20). The eluent of the desired fraction was evaporated, yielding 18.1 parts (67.3%) of [3-(dimethoxymethyl)-4-nitrophenyl]phenylmethanone (interm. 10).

후처리

  1. customwhile bubbling air through it
  2. additionThe reaction mixture was poured into water
  3. extractionthe whole was extracted with dichloromethane
  4. customThe extract was dried
  5. filtrationfiltered
  6. customevaporated
  7. customthe residue was purified by column chromatography (silica gel; CHCl3 /hexane 80:20)
  8. customThe eluent of the desired fraction was evaporated

출처 및 근거

ORD 기록
ord-fa2624b870434a03b915e85e110280e0
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05037829

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