p-Toluenesulfonic acid monohydrate → p-Toluenesulfonic acid
反応式
N1C=CC(CN2CCCNC2=C[N+]([O-])=O)=CC=1.O.[C:19]1([CH3:29])[CH:24]=[CH:23][C:22]([S:25]([OH:28])(=[O:27])=[O:26])=[CH:21][CH:20]=1>CC(C)=O.C(Cl)(Cl)Cl>[CH3:29][C:19]1[CH:24]=[CH:23][C:22]([S:25]([OH:28])(=[O:27])=[O:26])=[CH:21][CH:20]=1参加物
5
実験手順
Compound No. 1 (0.73 g) obtained in Example 1 was dissolved in a mixed solvent of acetone (10 ml) and chloroform (50 ml), and p-toluenesulfonic acid hydrate (0.63 g) was added. The mixture was vigorously shaken for 2 hours, and then allowed to stand at room temperature for 3 hours. The precipitated crystals were collected by filtration, and fully washed with acetone to give the p-toluenesulfonate (1.2 g) of compound No. 1 of this invention. mp. 170°-176° C.
後処理
- additionwas added
- waitto stand at room temperature for 3 hours
- filtrationThe precipitated crystals were collected by filtration
- washfully washed with acetone
出典と根拠
- ORDレコード
- ord-320b7e5e8b3245f3bef16df40e9ff193
- 出典データセット
- uspto-grants-1987_07
- 特許番号
- US04680294
反応ノート
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