反应详情

温度

100 °C

A glass microwave reaction vessel was charged with 2-chloro-8-iodo-3-(3-(methylsulfonyl)propyl)quinazolin-4(3H)-one (50 mg, 0.117 mmol) and tert-butylamine (0.123 mL, 1.172 mmol) in DMSO (0.5 mL). The reaction mixture was stirred and heated in an Initiator microwave reactor (Personal Chemistry, Biotage AB, Inc., Upssala, Sweden) at 100° C. for 1 h. The reaction was repeated on 150 mg scale. The reaction mixture were combined and diluted with water (20 mL). The mixture was extracted with CHCl3/iPrOH (4:1, 40 mL×3) and the combined organic layers were washed with water, dried (MgSO4), filtered and concentrated. The residue was purified with silica gel chromatography (eluted with 10-70% EtOAc in Hexanes) to give 2-(tert-butylamino)-8-iodo-3-(3-(methylsulfonyl)propyl)quinazolin-4(3H)-one (108 mg, 50% yield) as a yellow solid. MS (ESI, pos. ion) m/z: 464 (M+1).

1. customA glass microwave reaction vessel
2. extractionThe mixture was extracted with CHCl3/iPrOH (4:1, 40 mL×3)
3. washthe combined organic layers were washed with water
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified with silica gel chromatography (eluted with 10-70% EtOAc in Hexanes)