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

HRID 52145ノート

反応式

HRID 52145 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-10b0818619754d50a17613f7474b2253
出典データセット
uspto-grants-1997_04
特許番号
US05616581

反応ノート

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