Ethanol → Ethyl 3-(2,4-difluorophenylthio)-4-nitrobenzoate

HRID 1087174ノート

反応式

HRID 1087174 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[S:9][C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][C:18]=1[N+:19]([O-:21])=[O:20])[C:13]([OH:15])=[O:14].[CH2:22](O)[CH3:23]>Cl>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[S:9][C:10]1[CH:11]=[C:12]([CH:16]=[CH:17][C:18]=1[N+:19]([O-:21])=[O:20])[C:13]([O:15][CH2:22][CH3:23])=[O:14]

参加物

4

反応物 2

HCID 702EthanolHCID 100867683-(2,4-Difluorophenylthio)-4-nitrobenzoic acid

生成物 1

HCID 10359815Ethyl 3-(2,4-difluorophenylthio)-4-nitrobenzoate

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of 3-(2,4-difluorophenylthio)-4-nitrobenzoic acid (1.2 g) in 20% hydrogen chloride in ethanol (3 ml) was refluxed for 2 hours. The mixture was concentrated. The residue was dissolved in ethyl acetate and washed with an aqueous solution of sodium bicarbonate and water successively. The extract was evaporated and the residual oil was crystallized from a mixture of hexane and ethanol to give crystals of ethyl 3-(2,4-difluorophenylthio)-4-nitrobenzoate (1.1 g).

後処理

  1. concentrationThe mixture was concentrated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with an aqueous solution of sodium bicarbonate and water successively
  4. customThe extract was evaporated
  5. customthe residual oil was crystallized from a mixture of hexane and ethanol

出典と根拠

ORDレコード
ord-21550f48741d48fda2cb1c5a0abf243d
出典データセット
uspto-grants-1991_07
特許番号
US05034417

反応ノート

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