Water → 4-Chloro-5-(trifluoromethyl)benzene-1,2-diamine

HRID 53783

반응식

HRID 53783 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:12]([F:15])([F:14])[F:13])[C:5]([Cl:11])=[CH:6][C:7]=1[N+:8]([O-])=O.Cl[Sn]Cl.O>C(O)C>[NH2:1][C:2]1[CH:3]=[C:4]([C:12]([F:15])([F:13])[F:14])[C:5]([Cl:11])=[CH:6][C:7]=1[NH2:8]

참가 물질

5

반응물 3

HCID 962WaterHCID 24479Stannous ChlorideHCID 27376454-Chloro-2-nitro-5-(trifluoromethyl)aniline

생성물 1

HCID 27734974-Chloro-5-(trifluoromethyl)benzene-1,2-diamine수율 71%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
90 °C

실험 절차

To a stirred mixture of 3-amino-6-chloro-4-nitrobenzotrifluoride (300 mg, 1.25 mmol) in ethanol (5 mL) was added SnCl2.2 H2O (1.40 g, 6.20 mmol) in one portion. The mixture was refluxed at 80° C. (oil bath, 90° C.) for 1 h and the solution was cooled to room temperature and ice water (20 g) was added. It was adjusted to pH=7 and extracted with ethyl acetate. The extract was dried over Mg2SO4 and evaporated to give 185 mg (71%) of 3,4-diamino-6-chlorobenzotrifluoride as a brown solid. 1H NMR (CDCl3): δ 3.404 (s, 2H); 3.717 (s, 2H); 6.754 (s, 1H); 6.974 (s, 1H).

후처리

  1. temperaturethe solution was cooled to room temperature
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over Mg2SO4
  4. customevaporated

출처 및 근거

ORD 기록
ord-f868b29587a64c158f258690e36c6f9f
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620979

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