(1,1'-Biphenyl)-3-carboxylic acid → 3-Biphenylmethanol

HRID 234118

반응식

HRID 234118 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C:13]2[CH:14]=[C:15]([CH:19]=[CH:20][CH:21]=2)[C:16](O)=[O:17])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>CCOCC>[OH:17][CH2:16][C:15]1[CH:14]=[C:13]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH:21]=[CH:20][CH:19]=1

참가 물질

4

반응물 2

HCID 12854(1,1'-Biphenyl)-3-carboxylic acidHCID 21226445Aluminium lithium hydride

생성물 1

HCID 6035563-Biphenylmethanol수율 77.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a suspension of 100 mg of lithium aluminum hydride in 20 mL of ether was added 500 mg 3-phenylbenzoic acid. The reaction mixture was stirred at room temperature overnight. After any excess lithium aluminum hydride was destroyed with water, the organic layer was washed successively with 25 mL aliquots of dilute hydrochloric acid, dilute sodium hydroxide and brine. The organic phase was dried over anhydrous sodium sulfate and the solvent removed by evaporation under reduced pressure to yield 360 mg of 3-hydroxymethylbiphenyl as a crystalline solid. This material was used in the next step without further purification.

후처리

  1. customAfter any excess lithium aluminum hydride was destroyed with water
  2. washthe organic layer was washed successively with 25 mL aliquots of dilute hydrochloric acid, dilute sodium hydroxide and brine
  3. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  4. customthe solvent removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-646f6f2096e64e6abfe05b7d07f31e69
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594141

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