反应详情

温度

50 °C

A mixture of 4-benzyloxycarbonyl-1-[1-(tert-butoxycarbonyl)-4-piperidinylamino]-2-piperazinone (9.00 g), potassium carbonate (3.46 g) and methyl iodide (29.81 g) in DMF (100 ml) was stirred at 50° C. overnight. The reaction mixture was concentrated under reduced pressure, and the residue was combined with water (200 ml) and extracted with a mixture of ethyl acetate and tetrahydrofuran (1:1, 120 ml×3). The extract was washed with water and brine, dried and concentrated. The residue was crystallized from diisopropyl ether to obtain the title compound (8.55 g) as colorless crystals.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionextracted with a mixture of ethyl acetate and tetrahydrofuran (1:1, 120 ml×3)
3. washThe extract was washed with water and brine
4. customdried
5. concentrationconcentrated
6. customThe residue was crystallized from diisopropyl ether