反応式
[CH2:1]([NH:3][CH2:4][CH2:5][NH2:6])[CH3:2].[CH3:7][S:8]([NH:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([Cl:18])=[O:17])=[CH:14][CH:13]=1)(=[O:10])=[O:9]>O1CCCC1>[ClH:18].[CH2:1]([NH:3][CH2:4][CH2:5][NH:6][C:16](=[O:17])[C:15]1[CH:19]=[CH:20][C:12]([NH:11][S:8]([CH3:7])(=[O:10])=[O:9])=[CH:13][CH:14]=1)[CH3:2]参加物
4
実験手順
To a solution of 4.45 g (50.5 mmoles) of N-ethylethylenediamine in 50 ml of tetrahydrofuran cooled in an ice/ethanol bath under a nitrogen atmosphere add dropwise a solution of 11.8 g (50.5 mmoles) of 4-[(methylsulfonyl)amino]benzoyl chloride in 100 ml of tetrahydrofuran. When the addition is complete, allow the mixture to warm to room temperature and stir overnight. Filter the resulting solid and wash the solid with tetrahydrofuran then with diethyl ether. Triturate the solid in acetone, then recrystallize from 90% aqueous methanol to obtain the title compound.
後処理
- additionWhen the addition
- filtrationFilter the resulting solid
- washwash the solid with tetrahydrofuran
- customTriturate the solid in acetone
- customrecrystallize from 90% aqueous methanol
出典と根拠
- ORDレコード
- ord-48aa1403aa7244b387efc142af8ece4f
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04544654
関連ノート
読み込み中…