反应详情

温度

100 °C

To a solution of Formic acid (50 ml) and Formaldehyde solution (50 mL) was added 4-Nitro-1-pyrrolidin-3-yl-1H-pyrazole hydrochloride (10 g). The reaction mixture was heated at 100° C. for 16 h. The reaction mixture was concentrated under reduced pressure. The residue was tarturated with acetonitrile (150 mL), filtered off solid and filtrate was concentrated. The crude material was basified with ammonia solution, extracted with ethyl acetate, dried over sodium sulphate and evaporated to afford (7 g, 78%) as pale yellow liquid. 1H NMR (400 Mz, DMSO-d6) δ 8.85 (s, 1H), 8.24 (s, 1H), 5.24 (m, 1H), 2.75-2.81 (m, 3H), 2.33-2.49 (m, 2H), 2.27 (s, 3H), 2.12 (m, 1H).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. filtrationfiltered off solid and filtrate
3. concentrationwas concentrated
4. extractionextracted with ethyl acetate
5. dry with materialdried over sodium sulphate
6. customevaporated
7. customto afford (7 g, 78%) as pale yellow liquid