Ammonia methanol → HCID 89484446, Verbindung
Reaktionsgleichung
[NH3:1].CO.[S:4]1[CH:8]=[CH:7][C:6]2[C:9]([NH:13][C:14]3[N:15]=[C:16]([NH:25][C@@H:26]4[CH2:31][CH2:30][CH2:29][CH2:28][C@@H:27]4[NH:32]C(OC(C)(C)C)=O)[N:17]=[N:18][C:19]=3[C:20](OCC)=[O:21])=[CH:10][CH:11]=[CH:12][C:5]1=2>>[NH2:32][C@H:27]1[CH2:28][CH2:29][CH2:30][CH2:31][C@H:26]1[NH:25][C:16]1[N:17]=[N:18][C:19]([C:20]([NH2:1])=[O:21])=[C:14]([NH:13][C:9]2[C:6]3[CH:7]=[CH:8][S:4][C:5]=3[CH:12]=[CH:11][CH:10]=2)[N:15]=1Komponenten
3
Versuchsvorschrift
A 7 M ammonia-methanol solution (2 ml) was added to ethyl 5-(benzo[b]thiophen-4-ylamino)-3-((1R,2S)-2-(tert-butoxycarbonylamino)cyclohexylamino)-1,2,4-triazine-6-carboxylate obtained in the above-described Step 2 (71.8 mg), and then the reaction solution was allowed to react in a microwave reactor at 130° C. for 1 hour. The solvent was evaporated under vacuum, then trifluoroacetic acid (0.5 ml) was added to the resultant residue, and the reaction solution was stirred at room temperature for 5 minutes. The solvent was evaporated under vacuum, and then the resultant residue was purified by column chromatography on basic silica gel (developing solvent:hexane/ethyl acetate) to obtain the titled compound as a white solid.
Aufarbeitung
- customobtained in the above-described Step 2 (71.8 mg)