Thiophosgene → 2-Fluoro-1-isothiocyanato-3-trifluoromethyl-benzene

HRID 645567

반응식

HRID 645567 반응식
[F:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[NH2:12].C(=O)(O)[O-].[Na+].[C:18](Cl)(Cl)=[S:19]>ClCCl.O>[F:1][C:2]1[C:7]([C:8]([F:10])([F:11])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[N:12]=[C:18]=[S:19]

참가 물질

6

반응물 3

HCID 10040ThiophosgeneHCID 1455693-Amino-2-fluorobenzotrifluorideHCID 516892Sodium Bicarbonate

생성물 1

HCID 834024072-Fluoro-1-isothiocyanato-3-trifluoromethyl-benzene수율 91%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a two phase solution of 2-fluoro-3-trifluoromethyl-phenylamine (2 g, 11.17 mmole) in dichloromethane (40 ml) and sodium bicarbonate (6.57 g, 78.19 mmole) in water (30 ml) at 0° C. was added dropwise a solution of thiophosgene (1.28 g, 11.17 mmole) in dichloromethane (10 ml). After 2 hrs, the organic layer was separated, washed sequentially with 1M NaHCO3, brine and water. The organic layer was dried over Na2SO4, filtered and concentrated to yield 2.2 g (91%) of product as a viscous liquid. MS (ESI+) m/z 221 (M+H)+.

후처리

  1. customthe organic layer was separated
  2. washwashed sequentially with 1M NaHCO3, brine and water
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cf0ee22f5cc94cfc926380c79a751eaf
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07704997B1

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