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

HRID 1512270

반응식

HRID 1512270 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-0bf394cc131742ba8fd832f0a48df0be
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217067B2

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