Methyl chloroacetate → HCID 19963012, 화합물

HRID 1720053노트

반응식

HRID 1720053 반응식
[CH3:1][C:2]1[C:3]([CH2:19][S:20][C:21]2[NH:25][C:24]3[CH:26]=[CH:27][CH:28]=[CH:29][C:23]=3[N:22]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][NH:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.Cl[CH2:31][C:32]([O:34][CH3:35])=[O:33].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:1][C:2]1[C:3]([CH2:19][S:20][C:21]2[NH:22][C:23]3[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=3[N:25]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][N:11]([CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:31][C:32]([O:34][CH3:35])=[O:33]

참가 물질

5

반응물 3

HCID 7295Methyl chloroacetateHCID 11430Potassium CarbonateHCID 199630842-((3-Methyl-4-(2-benzylaminoethylthio)pyridin-2-yl)methylthio)-1H-benzimidazole

생성물 1

HCID 19963012HCID 19963012, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2-((3-Methyl-4-(2-benzylaminoethylthio)pyridin-2-yl)-methylthio)-1H-benzimidazole (2 g) was dissolved in dimethylformamide and reacted with methyl chloroacetate (0.45 ml) in the presence of potassium carbonate (0.71 g) at 50°-60° C. After the completion of the reaction, the dimethylformamide was distilled away and the residue was extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous magnesium sulfate and the solvent was distilled away to give an oily product. The oily product was purified by column chromatography to give 2-((3-methyl-4-(2-(N-benzyl-N-methoxycarbonylmethylamino)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole.

후처리

  1. customAfter the completion of the reaction
  2. distillationthe dimethylformamide was distilled away
  3. extractionthe residue was extracted with ethyl acetate
  4. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled away
  6. customto give an oily product
  7. customThe oily product was purified by column chromatography

출처 및 근거

ORD 기록
ord-b8a99f97879e4088a3f91cf13a17bc65
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05504082

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