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

HRID 566640ノート

反応式

HRID 566640 の反応式
[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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 260Hydrogen BromideHCID 10176652HCID 10176652、化合物

生成物 1

HCID 101765072-[(trifluoromethyl)sulfanyl]phenol収率 46%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-2bc00ae97c54417b98120ae06393c8f8
出典データセット
uspto-grants-2001_01
特許番号
US06175042B1

反応ノート

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