反应详情

To a solution of 1,3-bis(tert-butoxycarbonyl)-2-(trifluoromethylsulfonyl)guanidine (22.3 g) in dichloromethane (100 ml) were added 4,5-diamino-1-methylpyrazole sulfuric acid salt (10 g) and triethylamine (33.2 ml) at 4° C., and the mixture was stirred at room temperature overnight. The reaction mixture was poured into a mixture of ethyl acetate and water. The aqueous layer was separated, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo. The concentrate was poured into acetonitrile, and the resulting precipitate was collected by filtration and dried in vacuo to give 5-amino-4-[2′,3′-bis(tert-butoxycarbonyl)guanidino]-1-methylpyrazole (11.62 g).

1. customThe aqueous layer was separated
2. washthe organic layer was washed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo
6. additionThe concentrate was poured into acetonitrile
7. filtrationthe resulting precipitate was collected by filtration
8. customdried in vacuo