Ammonium Chloride → Ethyl 4-amino-3-(2,4-difluorophenylthio)benzoate

HRID 1087175ノート

反応式

HRID 1087175 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:18]=[CH:19][C:20]=1[N+:21]([O-])=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14].[Cl-].[NH4+]>C(O)C.O.[Fe]>[NH2:21][C:20]1[CH:19]=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:11][C:10]=1[S:9][C:3]1[CH:4]=[CH:5][C:6]([F:8])=[CH:7][C:2]=1[F:1]

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 10359815Ethyl 3-(2,4-difluorophenylthio)-4-nitrobenzoate

生成物 1

HCID 10040979Ethyl 4-amino-3-(2,4-difluorophenylthio)benzoate収率 109.7%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A mixture of ethyl 3-(2,4-difluorophenylthio)-4-nitrobenzoate (1.1 g), iron powder (1.1 g) and ammonium chloride (0.11 g) in ethanol (10 ml) and water (5 ml) was stirred and refluxed for 1 hour. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was dissolved in ethyl acetate, washed with water, dried and evaporated to give crystals of ethyl 4-amino-3-(2,4-difluorophenylthio)benzoate (1.1 g).

後処理

  1. temperaturerefluxed for 1 hour
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with water
  6. customdried
  7. customevaporated

出典と根拠

ORDレコード
ord-43e5049a3d9746408a2f3f8067a9e773
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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