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

HRID 1512270ノート

反応式

HRID 1512270 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 834024072-Fluoro-1-isothiocyanato-3-trifluoromethyl-benzene収率 91%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-0bf394cc131742ba8fd832f0a48df0be
出典データセット
uspto-grants-2012_07
特許番号
US08217067B2

反応ノート

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