Methanol → HCID 68290013、化合物

HRID 878774ノート

反応式

HRID 878774 の反応式
[CH:1]1([C:5]([F:18])([F:17])[C:6]2[CH:16]=[CH:15][C:9]([C:10](OCC)=[O:11])=[CH:8][CH:7]=2)[CH2:4][CH2:3][CH2:2]1.CO.[BH4-].[Li+].O>O1CCCC1>[CH:1]1([C:5]([F:17])([F:18])[C:6]2[CH:16]=[CH:15][C:9]([CH2:10][OH:11])=[CH:8][CH:7]=2)[CH2:2][CH2:3][CH2:4]1

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 4148881Lithium borohydrideHCID 69437235Ethyl 4-(cyclobutyldifluoromethyl)benzoate

生成物 1

HCID 68290013HCID 68290013、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl 4-[cyclobutyl(difluoro)methyl]benzoate (synthesized by the method of WO2005/032465, 140 mg, 0.55 mmol) in tetrahydrofuran (5 mL) and methanol (112 μL, 2.76 mmol) was added lithium borohydride (60 mg, 2.75 mmol) at 0° C. The mixture was stirred at room temperature for 3 hours, and then to the reaction solution was added water at 0° C., and the mixture was extracted with ethyl acetate three times. The organic layer was combined, washed with water and saturated brine, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure to give a crude {4-[cyclobutyl(difluoro)methyl]phenyl}methanol (111 mg) as a colorless oil. The resultant was used in the next step without further purification.

後処理

  1. extractionthe mixture was extracted with ethyl acetate three times
  2. washwashed with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-acbebdb563bf4f3ebf18d0db0d05a71a
出典データセット
uspto-grants-2015_03
特許番号
US08987445B2

反応ノート

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