Toluene → 80854-57-5

HRID 2265114ノート

反応式

HRID 2265114 の反応式
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[CH:6][CH:5]=1)=O.[C:13](C=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([O:15][CH2:16][CH3:17])=[O:14].[C:38]1(C)C=CC=CC=1>>[N+:10]([C:7]1[CH:8]=[CH:9][C:4](/[C:2](/[CH3:38])=[CH:1]/[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:5][CH:6]=1)([O-:12])=[O:11]

参加物

4

反応物 3

HCID 1140TolueneHCID 7487p-NitroacetophenoneHCID 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester

生成物 1

HCID 614540480854-57-5収率 29%

実験手順

A toluene (90 ml) solution of 4-nitroacetophenone (2.0 g) and (carbethoxymethylidene)triphenylphosphorane (6.33 g) was stirred while refluxing under heating for 10 hours. After the solution was allowed to cool, the solvent was distilled off. The obtained residue was purified by column chromatography (6.25% ethyl acetate/n-hexane) to obtain Compound 19a (829 mg, 29%) as a white solid.

後処理

  1. temperaturewhile refluxing
  2. temperatureunder heating for 10 hours
  3. temperatureto cool
  4. distillationthe solvent was distilled off
  5. customThe obtained residue was purified by column chromatography (6.25% ethyl acetate/n-hexane)

出典と根拠

ORDレコード
ord-d698436e2133487c8add22e095a73a7e
出典データセット
uspto-grants-2010_12
特許番号
US07855300B2

反応ノート

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