HRID660365
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1-(3-Methoxypropyl)-6-nitro-1H-indazole (33 g, 0.14 mol) was dissolved in methanol (400 mL) and Raney Ni (7 g) was added. The reaction mixture was hydrogenated under an atmosphere of hydrogen at rt for about 2 h. When the starting material has been consumed, the reaction mixture was filtered and the filtrate was concentrated under reduced pressure to give 1-(3-methoxypropyl)-1H-indazol-6-amine (27 g, 94% yield) which was used in the next step without purification. 1H NMR (400 MHz, CDCl3): δ 7.84 (s, 1H), 7.51 (d, J=8.4 Hz, 1H), 6.73 (s, 1H), 6.67-6.65 (dd, J=6.8, 2.0 Hz, 1H), 4.36-4.33 (t, J=6.4 Hz, 2H), 4.30-3.80 (brs, 2H), 3.30 (s, 3H), 3.30-3.28 (m, 2H), 2.16-2.10 (m, 2H).
WORKUP
后处理
- customWhen the starting material has been consumed
- filtrationthe reaction mixture was filtered
- concentrationthe filtrate was concentrated under reduced pressure