Thiophosgene → 4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylisothiocyanate

HRID 33760

반응식

HRID 33760 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][C:6]=1[F:12].C(=O)(O)[O-].[Na+].[C:23](Cl)(Cl)=[S:24]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]=[C:23]=[S:24])=[CH:7][C:6]=1[F:12]

참가 물질

5

반응물 3

HCID 10040ThiophosgeneHCID 516892Sodium BicarbonateHCID 289727064-(2,5-Dichlorophenoxy)-3-fluoroaniline

생성물 1

HCID 597976634-(2,5-Dichloro-phenoxy)-3-fluoro-phenylisothiocyanate수율 97.4%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylamine (1.36 g, 5 mmol) was dissolved in 150 ml of chloroform and 100 ml of saturated aqueous sodium bicarbonate was added. To this biphasic mixture was added dropwise a solution of thiophosgene (0.39 ml, 5 mmol) in 30 ml of chloroform at room temperature with vigorous stirring. The mixture was stirred vigorously for 1 hour at room temperature. The bottom layer of the mixture was separated, and the aqueous layer was extracted twice with CHCl3. The combined organic solution was washed with water, dried over Mg2SO4 and evaporated to give 1.53 g (97.4%) of crude product used for next step without further purification.

후처리

  1. customThe bottom layer of the mixture was separated
  2. extractionthe aqueous layer was extracted twice with CHCl3
  3. washThe combined organic solution was washed with water
  4. dry with materialdried over Mg2SO4
  5. customevaporated

출처 및 근거

ORD 기록
ord-b997bf5941b9465ca8966a1a87240e14
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429667B2

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