Acetic Acid → 2-[(trifluoromethyl)sulfanyl]phenol

HRID 566640노트

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HRID 566640 반응식
[F:1][C:2]([S:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12]C)([F:4])[F:3].Br.C(O)(=O)C>O>[F:1][C:2]([S:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[OH:12])([F:4])[F:3]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 260Hydrogen BromideHCID 10176652HCID 10176652, 화합물

생성물 1

HCID 101765072-[(trifluoromethyl)sulfanyl]phenol수율 46%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 4.69 g of 2-methoxyphenyl trifluoromethyl sulfide, obtained according to Example 3, 20 ml of 48% strength by weight aqueous hydrobromic acid, and 20 ml of 96% strength by weight acetic acid was boiled under reflux for 24 hours. The completion of the reaction was then checked by gas chromatography. After cooling, the reaction mixture was poured into water. The organic phase was separated off and the aqueous phase was extracted with dichloromethane. The extract was combined with the organic phase. Drying over magnesium sulfate, concentration, and vacuum distillation gave 2.01 g (46% of theory) of 2-hydroxyphenyl trifluoromethyl sulfide (boiling point 65-66° C. at 26 mbar, melting point 35-37° C.).

후처리

  1. customobtained
  2. temperatureunder reflux for 24 hours
  3. temperatureAfter cooling
  4. customThe organic phase was separated off
  5. extractionthe aqueous phase was extracted with dichloromethane
  6. dry with materialDrying over magnesium sulfate, concentration, and vacuum distillation

출처 및 근거

ORD 기록
ord-2bc00ae97c54417b98120ae06393c8f8
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06175042B1

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