Ethyl chloroformate → ethyl 2-((3-methyl-4-(2-morpholinoethylthio)-2-pyridyl)methylthio)-1H-benzimidazole1-carboxylate

HRID 52145노트

반응식

HRID 52145 반응식
[CH3:1][C:2]1[C:3]([CH2:17][S:18][C:19]2[NH:23][C:22]3[CH:24]=[CH:25][CH:26]=[CH:27][C:21]=3[N:20]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1.[C:28](Cl)(=[O:32])[O:29][CH2:30][CH3:31].[H-].[Na+]>CN(C)C=O>[CH3:1][C:2]1[C:3]([CH2:17][S:18][C:19]2[N:20]([C:28]([O:29][CH2:30][CH3:31])=[O:32])[C:21]3[CH:27]=[CH:26][CH:25]=[CH:24][C:22]=3[N:23]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1

참가 물질

5

반응물 3

HCID 10928Ethyl chloroformateHCID 24758Sodium hydrideHCID 98492092-((3-methyl-4-(2-morpholinoethylthio)-2-pyridyl)methylthio)-1H-benzimidazole

생성물 1

HCID 15307532ethyl 2-((3-methyl-4-(2-morpholinoethylthio)-2-pyridyl)methylthio)-1H-benzimidazole1-carboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2-((3-Methyl-4-(2-morpholinoethylthio)-2-pyridyl)methylthio)-1H-benzimidazole (10 g) was reacted with 1.1 equivalents of ethyl chlorocarbonate in dimethylformamide in the presence of 1.1 equivalents of sodium hydride at room temperature. After the completion of the reaction, the solvent was distilled away and water was added to the residue, followed by extraction with chloroform. The chloroform layer was dried over anhydrous magnesium sulfate and the solvent was distilled away to give 11 g of ethyl 2-((3-methyl-4-(2-morpholinoethylthio)-2-pyridyl)methylthio)-1H-benzimidazole1-carboxylate as crystals, melting point 145°-147° C.

후처리

  1. customAfter the completion of the reaction
  2. distillationthe solvent was distilled away
  3. additionwater was added to the residue
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled away

출처 및 근거

ORD 기록
ord-10b0818619754d50a17613f7474b2253
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616581

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