反应详情

A mixture of 4-(5-iodo-1H-pyrazol-4-yl)-2-(methylthio)pyrimidine (A) (31.8 g, 0.1 mol), 2-iodo-propane (85 g, 50 mL, 0.5 mol) and K2CO3 (16.5 g, 0.12 mol) in DMF (500 mL) was heated at 40˜50° C. overnight. When TLC (hexane: EtOAc=15:1) showed the reaction was complete, DMF was evaporated under reduced pressure. The residue was taken up with EtOAc (400 mL). The mixture was washed with saturated aqueous NaCl, dried over Na2SO4 and concentrated to give crude product, which was purified via prep. HPLC to give pure 4-(3-iodo-1-isopropyl-1H-pyrazol-4-yl)-2-(methylthio)pyrimidine B-1-1 (17 g, 47.2%) as a yellow oil.

1. temperaturewas heated at 40˜50° C. overnight
2. customDMF was evaporated under reduced pressure
3. washThe mixture was washed with saturated aqueous NaCl
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customto give crude product, which
7. customwas purified via prep