Methanol → 4-(Hydroxymethyl)-3-(trifluoromethyl)phenol

HRID 1946307노트

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HRID 1946307 반응식
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](O)=[O:7])=[C:4]([C:11]([F:14])([F:13])[F:12])[CH:3]=1.CO>C1COCC1>[OH:7][CH2:6][C:5]1[CH:9]=[CH:10][C:2]([OH:1])=[CH:3][C:4]=1[C:11]([F:12])([F:13])[F:14]

참가 물질

4

반응물 2

HCID 887MethanolHCID 27751114-Hydroxy-2-(trifluoromethyl)benzoic acid

생성물 1

HCID 595479534-(Hydroxymethyl)-3-(trifluoromethyl)phenol수율 102%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

To a solution of 4-hydroxy-2-(trifluoromethyl)benzoic acid (4.62 g, 22.4 mmol, Fluorochem) in THF (60 ml) at ambient temperature under nitrogen was added dropwise 1.0 M borane-tetrahydrofuran complex (48 ml, 48.0 mmol). The solution was heated to 80° C. for 2 h. To the solution at ambient temperature was added methanol dropwise (40 ml). The solution was heated to 80° C. for 30 min. The solvent was removed in vacuo and the residue dissolved in methanol (100 ml). The solvent was removed in vacuo to leave the title compound as a white solid (4.39 g);

후처리

  1. temperatureThe solution was heated to 80° C. for 30 min
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue dissolved in methanol (100 ml)
  4. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-c106a1be46754785b678e20e3d2e422d
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399436B2

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