Acetic Acid → HCID 14257101, 화합물

HRID 622114노트

반응식

HRID 622114 반응식
[C:1]([CH:6]=[CH:7][C:8]1[N:12]([CH3:13])[C:11]([S:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)=[N:10][C:9]=1[CH3:24])([O:3][CH2:4][CH3:5])=[O:2].N(C([O-])=O)=NC([O-])=O.[K+].[K+].C(O)(=O)C>CO>[C:1]([CH2:6][CH2:7][C:8]1[N:12]([CH3:13])[C:11]([S:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)=[N:10][C:9]=1[CH3:24])([O:3][CH2:4][CH3:5])=[O:2]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 6096233Potassium diazene-1,2-dicarboxylateHCID 54335975HCID 54335975, 화합물

생성물 1

HCID 14257101HCID 14257101, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 5-[2-(carbethoxy)ethenyl]-1,4-dimethyl-2-(4-methoxybenzylthio)imidazole (600 mg, 1.7 mmole) and potassium azodicarboxylate (29 g, 0.17 mole) in methanol (50 ml) was stirred and treated with acetic acid (7 g, 0.12 mole). The mixture was concentrated in vacuo, partitioned between methylene chloride and 5% aqueous sodium carbonate, and the organic phase was concentrated in vacuo. The residue was chromatographed on silica gel eluted with ethyl acetate to give 5-[2-(carbethoxy)ethyl]-1,4-dimethyl-2-(4-methoxybenzylthio)imidazole (mp 63° C.).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. custompartitioned between methylene chloride and 5% aqueous sodium carbonate
  3. concentrationthe organic phase was concentrated in vacuo
  4. customThe residue was chromatographed on silica gel
  5. washeluted with ethyl acetate

출처 및 근거

ORD 기록
ord-3e6e8d5b7af64071b1bcfc2688ee6149
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04769386

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