Water → (+)-4-Hydroxy-4'-(2-methylbutanoyl) biphenyl

HRID 846556

반응식

HRID 846556 반응식
CC(CC)C(O)=[O:4].[CH3:8][CH:9]([CH2:24][CH3:25])[C:10]([C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:14][CH:13]=1)=[O:11].O.C(=O)([O-])O.[Na+]>CO>[OH:4][C:21]1[CH:22]=[CH:23][C:18]([C:15]2[CH:16]=[CH:17][C:12]([C:10](=[O:11])[CH:9]([CH3:8])[CH2:24][CH3:25])=[CH:13][CH:14]=2)=[CH:19][CH:20]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 679137652-Methylbutanoic acid 4-(2-methylbutanoyl) biphenyl

생성물 1

HCID 14745904(+)-4-Hydroxy-4'-(2-methylbutanoyl) biphenyl수율 88%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

0.67 g of the above 2-methylbutanoic acid-4-(2-methylbutanoyl) biphenyl was mixed with 95 ml of methyl alcohol and 5 ml of water and added with 1.14 g (13.6 mmol) of sodium hydrogen carbonate with stirring, which was subjected to hydrolysis reaction at room temperature for 40 hours. After the completion of the reaction, methanol was distilled off and 1 normal hydrochloric acid was added to adjust pH to not more than 1, and the extraction with dichloromethane was performed. The extracted liquid was washed with water, dried on anhydrous sodium sulfate and purified by a column chromatography of silica gel after the removal of the solvent to obtain 0.44 g (yield 88%) of (+)-4-hydroxy-4'-(2-methylbutanoyl) biphenyl at a light yellow crystal having the aforementioned properties.

후처리

  1. customwhich was subjected to hydrolysis reaction at room temperature for 40 hours
  2. distillationwas distilled off
  3. addition1 normal hydrochloric acid was added
  4. extractionthe extraction with dichloromethane
  5. washThe extracted liquid was washed with water
  6. dry with materialdried on anhydrous sodium sulfate
  7. custompurified by a column chromatography of silica gel
  8. customafter the removal of the solvent

출처 및 근거

ORD 기록
ord-4b8fb10e80624a48ad53c387e8cec10a
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05137653

연결된 노트

불러오는 중…