반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:14]3[C:15]([CH3:19])=[C:16]([CH3:18])[S:17][C:13]=3[N:12]3[C:20]([CH3:23])=[N:21][N:22]=[C:11]3[C@H:10]([CH2:24][C:25](O)=[O:26])[N:9]=2)=[CH:4][CH:3]=1.[CH2:28]([N:30](CC)CC)C.C(Cl)(=O)C(C)(C)C.CN>CN(C)C=O.O.O1CCCC1>[CH3:28][NH:30][C:25](=[O:26])[CH2:24][C@@H:10]1[N:9]=[C:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[C:14]2[C:15]([CH3:19])=[C:16]([CH3:18])[S:17][C:13]=2[N:12]2[C:20]([CH3:23])=[N:21][N:22]=[C:11]12참가 물질
반응물 4
생성물 1
시약·촉매·용매 3
반응 조건
- 온도
- -5 °C
실험 절차
(S)-4-(4-Chlorophenyl)-2,3,9-trimethyl-6H-thieno[3,2-f]-[1,2,4]triazolo[4,3-a][1,4]diazepine-6-acetic acid (7.0 g) and triethylamine (2.73 ml) are added to a mixed solvent of dimethylformamide (70 ml) and tetrahydrofuran (30 ml). The mixture is cooled to -5° C., and pivaloyl chloride (2.38 ml) is dropwise added at said temperature. Ten minutes later, a solution of methylamine (0.69 g) in dimethylformamide (5 ml) is dropwise added at said temperature, and the mixture is stirred at room temperature for 2 hours. Water is added to the reaction mixture, and the mixture is extracted with ethyl acetate, washed with water and dried over anhydrous magnesium sulfate. The solvent is distilled away, and the residue is recrystallized from water/methanol to give 2.29 g of (S)-N-methyl-4-(4-chloro-phenyl)-2,3,9-trimethyl-6H-thieno[3,2-f][1,2,4]triazolo[4,3-a]-[1,4]diazepine-6-acetamide 1/4 hydrate, melting point 143°-145° C.
후처리
- extractionthe mixture is extracted with ethyl acetate
- washwashed with water
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe solvent is distilled away
- customthe residue is recrystallized from water/methanol
출처 및 근거
- ORD 기록
- ord-a9af79cf68fe44bd955b58f6d97777a8
- 출처 데이터셋
- uspto-grants-1998_01
- 특허 번호
- US05712274
연결된 노트
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