Water → 2-Chloro-4-((1,1-dimethylethyl)thio)benzenamine

HRID 2072593노트

반응식

HRID 2072593 반응식
CN(C)C1CCCCC1.[Cl:10][C:11]1[CH:17]=[C:16]([SH:18])[CH:15]=[CH:14][C:12]=1[NH2:13].[C:19](Br)([CH3:22])([CH3:21])[CH3:20].O>C(Cl)Cl>[Cl:10][C:11]1[CH:17]=[C:16]([S:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH:15]=[CH:14][C:12]=1[NH2:13]

참가 물질

6

반응물 4

HCID 962WaterHCID 7415N,N-Dimethylcyclohexylamine2회HCID 10485t-Butyl bromide2회HCID 198585664-Amino-3-chlorobenzenethiol

생성물 1

HCID 150638442-Chloro-4-((1,1-dimethylethyl)thio)benzenamine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Dimethylcyclohexylamine (22.86 g., 0.18 mole) in methylene chloride (125 ml.) is added dropwise to a stirred solution of 2-chloro-4-mercaptoaniline (27.0 g., 0.17 mole) and tert-butyl bromide (22.86 g., 0.18 mole) in methylene chloride (125 ml.) and the mixture is allowed to stir at room temperature for about 68 hours. An additional quantity of dimethylcyclohexylamine (2.3 g.) and tert-butyl bromide (2.5 g., 0.018 mole) is added and stirring is continued overnight. The reaction is poured into water, and the product is extracted with methylene chloride. The combined extracts are washed with dilute hydrochloric acid, water and dried. Removal of the drying agent and methylene chloride gives impure 2-chloro-4-tert-butylthioaniline as a beige solid.

후처리

  1. stirringstirring
  2. waitis continued overnight
  3. extractionthe product is extracted with methylene chloride
  4. washThe combined extracts are washed with dilute hydrochloric acid, water
  5. customdried
  6. customRemoval of the drying agent and methylene chloride

출처 및 근거

ORD 기록
ord-a09d16db94f1471c959bd28658b35775
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04913728

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