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

HRID 2247888ノート

反応式

HRID 2247888 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fa2624b870434a03b915e85e110280e0
出典データセット
uspto-grants-1991_08
特許番号
US05037829

反応ノート

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