Trifluoroacetic acid → (+/-)-N-[7-((4aR*,8aS*)-2-amino-4,4a,5,6-tetrahydro-7-oxa-3-thia-1-azanaphthalen-8a-yl)-2,2-difluorobenzo[1,3]dioxol-5-yl]-5-cyanopyridine-2-carboxamide

関与物質

反応手順

5-Cyanopyridine-2-carboxylic acid (4.0 mg), diisopropylethylamine (11.5 μl) and PyBOP (17.6 mg) were added to a solution of tert-butyl (±)-[(4aR*,8aS*)-8a-(6-amino-2,2-difluorobenzo[1,3]dioxol-4-yl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate (10 mg) in dichloromethane (2.0 ml) in an ice bath. The mixture was heated to room temperature and stirred for four hours. The solvent was evaporated under reduced pressure and the residue was purified by NH-pTLC to obtain an intermediate. The resulting intermediate was dissolved in dichloromethane (3.0 ml) and TFA (1.0 ml) was added. After stirring at room temperature for four hours, the reaction solution was diluted with water and neutralized with a sodium bicarbonate solution. The aqueous layer was extracted with dichloromethane, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by NH-pTLC to obtain the title compound.

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