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

HRID 1087175노트

반응식

HRID 1087175 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-43e5049a3d9746408a2f3f8067a9e773
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034417

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