p-Toluenesulfonic acid monohydrate → p-Toluenesulfonic acid
반응식
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]=1참가 물질
5
실험 절차
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 hour. 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.
후처리
- additionwas added
- waitto stand at room temperature for 3 hour
- filtrationThe precipitated crystals were collected by filtration
- washfully washed with acetone
출처 및 근거
- ORD 기록
- ord-660a043b23034f939d0612f5859939fd
- 출처 데이터셋
- uspto-grants-1987_03
- 특허 번호
- US04647570
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