Water → 4-[2-[[1,1'-Biphenyl]-2-yl]-2-oxoethoxy]-alpha-oxobenzeneacetic acid

HRID 2225846노트

반응식

HRID 2225846 반응식
C[O:2][C:3](=[O:28])[C:4](=[O:27])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[O:14])=[CH:7][CH:6]=1.[OH-].[Na+].O>CO>[C:16]1([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[C:13](=[O:14])[CH2:12][O:11][C:8]1[CH:9]=[CH:10][C:5]([C:4](=[O:27])[C:3]([OH:28])=[O:2])=[CH:6][CH:7]=1

참가 물질

5

실험 절차

A solution of 4-[-2-[[1,1'-biphenyl]-2-yl]-2-oxoethoxy]-alpha-oxobenzeneacetic acid methyl ester (0.563 g) in warm methanol (5 mL) was treated with 1N sodium hydroxide (3.3 mL). Within 5 minutes water (30 mL) was added, then after the methanol was removed in vacuo, the mixture was acidified with 1N hydrochloric acid (4.1 mL) and extracted with dichloromethane (1×60 mL, 2×10 mL). The combined organic layers were washed with water, then dried (MgSO4) and evaporated. The resulting yellow foam was taken up in diethyl ether, and after the the mixture was filtered to remove some insoluble material, the fillrate was evaporated and the residue was lyophilized from benzene to furnish 0.36 g of 4-[2-[[1,1'-biphenyl]-2-yl]-2-oxoethoxy]-alpha-oxobenzeneacetic acid.

후처리

  1. customafter the methanol was removed in vacuo
  2. extractionextracted with dichloromethane (1×60 mL, 2×10 mL)
  3. washThe combined organic layers were washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. filtrationafter the the mixture was filtered
  7. customto remove some insoluble material
  8. customthe fillrate was evaporated

출처 및 근거

ORD 기록
ord-c75670e30abd40af91c3de1f0471ec3f
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05344843

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