反应详情

A solution of 120 mg (5.0 mmol) LiOH in 5 mL water was metered into a solution of 1.0 g (1.8 mmol) (R)-2-(4-amino-3-methyl-5-nitro-phenyl)-1-methoxy-carbonyl-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 10 mL THF, the reaction solution was stirred for 4 h at RT and then evaporated down i.vac. The residue was combined with 30 mL water, washed with 30 mL diethyl ether, acidified with 4 M HCl while cooling with an ice bath and stirred for 30 min at RT. The precipitate was filtered off, washed with water and dried.

1. customevaporated down i.vac
2. washwashed with 30 mL diethyl ether
3. temperaturewhile cooling with an ice bath
4. stirringstirred for 30 min at RT
5. filtrationThe precipitate was filtered off
6. washwashed with water
7. customdried