反应详情

A stirred solution of 7-ethyl-2-isopropyl-2-methyl-5H-imidazo[1′,2′:1,2]pyrrolo[3,4-b]pyridine-3(2H),5-dione (7.25 g, 26.75 mmol) in anhydrous N,N-dimethylformamide is treated successively with methyl 6-aminocaproate hydrochloride (5.10 g, 28.1 mmol) and triethylamine (3.00 g, 29.6 mmol). The resulting mixture is stirred at room temperature under nitrogen for 20.5 hours. After this period, the reaction mixture is partitioned between water and ethyl acetate. The layers are separated, and the organic layer is washed with water, dried over magnesium sulfate and vacuum filtered through diatomaceous earth. The filtrate is concentrated in vacuo to obtain a white solid. The solid is triturated with 1:1 ether/petroleum ether to give the title product as a white solid (7.40 g, 69%, mp 101-103° C.).

1. waitAfter this period
2. customthe reaction mixture is partitioned between water and ethyl acetate
3. customThe layers are separated
4. washthe organic layer is washed with water
5. dry with materialdried over magnesium sulfate and vacuum
6. filtrationfiltered through diatomaceous earth
7. concentrationThe filtrate is concentrated in vacuo
8. customto obtain a white solid
9. customThe solid is triturated with 1:1 ether/petroleum ether