Acetic Acid → HCID 14257101、化合物

HRID 622114ノート

反応式

HRID 622114 の反応式
[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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 6096233Potassium diazene-1,2-dicarboxylateHCID 54335975HCID 54335975、化合物

生成物 1

HCID 14257101HCID 14257101、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-3e6e8d5b7af64071b1bcfc2688ee6149
出典データセット
uspto-grants-1988_09
特許番号
US04769386

反応ノート

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