反応式
[CH3:1][C:2]1([CH3:9])[NH:6][C:5](=[O:7])[NH:4][C:3]1=[O:8].Cl[CH2:11][CH2:12][CH2:13][CH2:14][S:15][C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1.C1CCN2C(=NCCC2)CC1.C(OCC)(=O)C>CN(C)C=O>[CH3:1][C:2]1([CH3:9])[NH:6][C:5](=[O:7])[N:4]([CH2:11][CH2:12][CH2:13][CH2:14][S:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[C:3]1=[O:8]参加物
6
実験手順
To a solution of 2.56 g (20 mmol) of 5,5-dimethylhydantoin and 4.03 g (20 mmol) of 4-(4-chlorobutylthio)pyridine in 20 ml of N,N-dimethylformamide, 3.00 ml (20 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene was added, and the mixture was stirred at room temperature for 43 hours, followed by further stirring at 70° C. for 10 hours. Ethyl acetate was added to the reaction mixture, and the mixture was washed three times with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/ethanol =10:1) to give 3.33 g of the desired compound (56.8% yield, colorless crystals).
後処理
- stirringby further stirring at 70° C. for 10 hours
- washthe mixture was washed three times with water
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off
- customthe residue was purified by column chromatography (eluent: ethyl acetate/ethanol =10:1)
出典と根拠
- ORDレコード
- ord-223b53ba401c4783b307cafc7579f4f4
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05246948
関連ノート
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