反応式
[C:1]([O:4][C:5]1[C:6](=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:7](Cl)=[O:8])(=[O:3])[CH3:2].[CH3:14][S:15][C:16]1[S:20][C:19]([NH2:21])=[N:18][CH:17]=1.C(N(CC)CC)C>C1COCC1>[C:1]([O:4][C:5]1[CH:13]=[CH:12][CH:11]=[CH:10][C:6]=1[C:7](=[O:8])[NH:21][C:19]1[S:20][C:16]([S:15][CH3:14])=[CH:17][N:18]=1)(=[O:3])[CH3:2]参加物
実験手順
Under nitrogen a solution of acetylsalicyloyl chloride (1.237 g, 6.20 mmol, 1.3 eq) in THF (40 mL) was added to a stirred solution of 5-(methylthio)thiazol-2-amine ? (700.0 mg, 4.79 mmol, 1.0 eq) in dry THF (mL). This was followed by the addition of triethylamine (0.67 mL, 4.79 mmol, 1.0 eq). The reaction mixture was stirred at room temperature and monitored by TLC. After two hours, reaction was filtered through sintered funnel and solvent removed in vacuo. The crude product was dissolved in EtOAc (150 mL) and washed twice each with 1M HCl and saturated aq. sodium hydrogen carbonate solutions. The organic fraction was dried over MgSO4 followed the removal of solvent. Flash column chromatography yielded the pure product 69 (1.450 g, 98%) as a solid.
後処理
- customreaction
- filtrationwas filtered through sintered funnel
- customsolvent removed in vacuo
- dissolutionThe crude product was dissolved in EtOAc (150 mL)
- washwashed twice each with 1M HCl and saturated aq. sodium hydrogen carbonate solutions
- dry with materialThe organic fraction was dried over MgSO4
- customthe removal of solvent
出典と根拠
- ORDレコード
- ord-ccd6077007a54d03ad394d9cafe2fcfd
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08895752B2
関連ノート
読み込み中…