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Benzil → 3-(4,5-diphenyl-1H-imidazol-2-yl)propionic acid methyl ester

HRID 220261
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인쇄 미리보기

반응식

HRID 220261 반응식
[C:1]1([C:7]([C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=O)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:17][O:18][CH:19]([O:26]C)[CH2:20][CH2:21][C:22](OC)=O.C([O-])(=O)C.[NH4+:32].[OH-].[NH4+:34]>C(O)(=O)C.O>[CH3:17][O:18][C:19](=[O:26])[CH2:20][CH2:21][C:22]1[NH:32][C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8651BenzilHCID 14923Ammonium HydroxideHCID 350846Methyl 4,4-dimethoxybutanoateHCID 517165Ammonium Acetate

생성물 1

HCID 684138073-(4,5-diphenyl-1H-imidazol-2-yl)propionic acid methyl ester

시약·촉매·용매 2

HCID 176Acetic Acid용매
HCID 962
Water
용매

실험 절차

A solution of 1 g of benzil, 1.01 g of methyl 4,4-dimethoxybutyrate and 2.87 g of ammonium acetate in 23 mL of acetic acid was refluxed for 5 h. The mixture was poured into water, basified with a 25% aq. ammonium hydroxide solution and extracted with DCM. The organic phase was dried over anh. Na2SO4 and concentrated in vacuo. The resulting crude material was purified by CC using heptane/EtOAc from 85/15 to 0/100 as eluant to yield 633 mg of 3-(4,5-diphenyl-1H-imidazol-2-yl)-propionic acid methyl ester as a yellowish solid.

후처리

  1. extractionextracted with DCM
  2. dry with materialThe organic phase was dried over anh. Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe resulting crude material was purified by CC

출처 및 근거

ORD 기록
ord-892bcec21f6c40609c2057332dd0077b
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202885B2

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