反应详情

温度

100 °C

A mixture of water (430 mL) and 37% HCl in water (299.9 mL, 3.65 mol) is added to a suspension of di-tert-butyl (1S,2R,3S,4S,5R,6R)-2-[(tert-butoxycarbonyl)amino]-3-[(3,4-dichlorobenzyl)oxy]-4-hydroxybicyclo[3.1.0]hexane-2,6-dicarboxylate (215 g, 365.3 mmol) in 1,4-dioxane (73.1 mL). The resulting slurry is stirred at 100° C. for 4.5 hours, cooled to 25° C. and concentrated in vacuo to provide a white solid. Triturate sequentially with methyl tert-butyl ether (2 L) and hexanes (2 L) and then filter to collect the solids. Dry under vacuum for 16 hours. The solid is washed again with methyl tert-butyl ether (2×1 L) and hexane (1 L), then dried under vacuum at 50° C. overnight to yield the title compound as a white solid (140.4 g, 93% yield). MS (m/z): 376/378 (M+1).

1. temperaturecooled to 25° C.
2. concentrationconcentrated in vacuo
3. customto provide a white solid
4. customTriturate sequentially with methyl tert-butyl ether (2 L) and hexanes (2 L)
5. filtrationfilter
6. customto collect the solids
7. customDry under vacuum for 16 hours
8. washThe solid is washed again with methyl tert-butyl ether (2×1 L) and hexane (1 L)
9. customdried under vacuum at 50° C. overnight