反应详情

温度

50 °C

To a ethanol solution (20 ml) of tert-butyl(1-ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-yl)methyl((2-(hydroxymethyl)pyridin-3-yl)methyl)carbamate (0.82 g) was added 5 M HCl and the mixture was stirred at 50° C. for 7 hours. The resulting mixture was concentrated and then 5 M NaOH was added thereto. Organic materials were extracted with ethyl acetate twice and then dried over MgSO4. After evaporation, the residue was purified by column chromatography (methanol/ethyl acetate 1:9→1:1) to give the titled compound as pale yellow oil (0.37 g).

1. concentrationThe resulting mixture was concentrated
2. addition5 M NaOH was added
3. extractionOrganic materials were extracted with ethyl acetate twice
4. dry with materialdried over MgSO4
5. customAfter evaporation
6. customthe residue was purified by column chromatography (methanol/ethyl acetate 1:9→1:1)