反应详情

温度

80 °C

A solution of 3-[1-(1-hydroxyprop-3-yl)-4-piperidinyl]-6-fluoro-1H-indazole (230 mg, 0.83 mmol) in 5 ml dry DMF was added 3,4-methylenedioxyphenylisocyanate (291 mg, 1.65 mmol) in 3 ml dry DMF. The reaction was heated to 100° C. for 2 h and 16 h at 80° C. The reaction was cooled to room temperature and added a mixture of 50 ml water and 200 ml ether, filtered and separated. The ether phase was washed with water, brine and dried with sodium sulphate and concentrated in vacuo. The crude product was purified by chromatography on silica gel 60 eluting with ethyl acetate:methanol (9:1, v/v). Concentration of the appropriate fractions afforded 50 mg (11%) of the title compound as an amorphous solid.

1. temperatureThe reaction was cooled to room temperature
2. additionadded
3. filtrationfiltered
4. customseparated
5. washThe ether phase was washed with water, brine
6. dry with materialdried with sodium sulphate
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by chromatography on silica gel 60 eluting with ethyl acetate:methanol (9:1