异丙胺 → 1,4-dichloro-6-isopropyl-6H-pyrrolo[3,4-d]pyridazine

温度

70 °C

To a suspension of 4,5-bis(bromomethyl)-3,6-dichloropyridazine (700 mg, 2.09 mmol) in 66 mL anhydrous THF was added with sodium carbonate (443 mg, 4.18 mmol) and tetrabutylammonium iodide (77.2 mg, 0.21 mmol). The reaction mixture was added with isopropyl amine (0.18 mL, 2.09 mmol) in 10 mL THF dropwisely for 2 h. The reaction mixture was heated at 70° C. for 3 h. The reaction mixture was concentrated, dissolved in DCM and washed with water and brine. The organics solution was dried over Na2SO4 and concentrated to afford a crude oil. The mixture was purified by flash chromatography on silica gel, eluting with 10-80% EtOAc:heptane to afford a off-white solid (280 mg, yield: 47%).

1. concentrationThe reaction mixture was concentrated
2. dissolutiondissolved in DCM
3. washwashed with water and brine
4. dry with materialThe organics solution was dried over Na2SO4
5. concentrationconcentrated
6. customto afford a crude oil
7. customThe mixture was purified by flash chromatography on silica gel
8. washeluting with 10-80% EtOAc

ORD记录

ord-9441bd98ad47423c9bcb6f925b4f2f6c

来源数据集

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

专利号

US08536168B2