Water → 4-Bromo-2-(trifluoromethyl)benzenethiol

HRID 1697492노트

반응식

HRID 1697492 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=O)=O)=[C:4]([C:12]([F:15])([F:14])[F:13])[CH:3]=1.O.Cl.C(CCP(CCC(O)=O)CCC(O)=O)(O)=O>O1CCOCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[C:4]([C:12]([F:15])([F:13])[F:14])[CH:3]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 2734570Tris(2-carboxyethyl)phosphine hydrochlorideHCID 27786084-Bromo-2-(trifluoromethyl)benzenesulfonyl chloride

생성물 1

HCID 509979974-Bromo-2-(trifluoromethyl)benzenethiol수율 99.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To as solution of 4-bromo-2-trifluoromethyl-benzenesulfonyl chloride (4.85 g) in dioxane (29 ml) was added at 22° C. water (6.5 ml) and tris-(2-carboxyethyl)phosphine hydrochloride (17.3 g) and the mixture was heated to reflux temperature for 6 h. The cooled mixture was partitioned between water and dichloromethane, the organic layer was washed with water, dried and evaporated give pure 4-bromo-2-trifluoromethyl-benzenethiol (3.85 g) as a colorless liquid. MS: 257.2 and 255.1 [M−H]−.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux temperature for 6 h
  3. customThe cooled mixture was partitioned between water and dichloromethane
  4. washthe organic layer was washed with water
  5. customdried
  6. customevaporated

출처 및 근거

ORD 기록
ord-b382cba9c4c4412ca9ea37e9ae17a398
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163793B2

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