反应详情

温度

23 °C

To a solution of (1aR,5aR)-2-(4-bromo-pyridin-2-yl)-1a,2,5,5a-tetrahydro-1H-2,3-diaza-cyclopropa[a]pentalene-4-carboxylic acid ethyl ester (9.0 g, 25.8 mmol) in THF (50 mL) and MeOH (50.0 mL) was added a 2.0 M aqueous solution of sodium hydroxide (25.8 mL, 51.7 mmol). The reaction was stirred at 23° C. for 2 h then concentrated to remove the organic solvents. The remaining residue was diluted to 150 mL with water. This solution was filtered to remove trace insoluble impurities then acidified to pH ˜3 with 6 M HCl. The resulting precipitate was collected by filtration, rinsed with water, then dried under vacuum to give the title compound (8.3 g) as a white solid. LCMS m/z=320.0 [M+H]+.

1. concentrationthen concentrated
2. customto remove the organic solvents
3. additionThe remaining residue was diluted to 150 mL with water
4. filtrationThis solution was filtered
5. customto remove trace insoluble impurities
6. filtrationThe resulting precipitate was collected by filtration
7. washrinsed with water
8. customdried under vacuum