反应详情

温度

90 °C

4-{2-Chloro-6-[(isopropylsulfonyl)methyl]pyrimidin-4-yl}morpholine (1.5 g, 4.69 mmol) was dissolved in a solution of 18% DMF in a mixture of 7:3:2 dimethoxyethane:water:ethanol (36 mL). {4-[(Tert-butoxycarbonyl)amino]phenyl}boronic acid (1.67 g, 7.04 mmol), 2M sodium carbonate solution (12 mL) and dichlorobis(triphenylphosphine) palladium catalyst (165 mg, 0.23 mmol) were then added and the reaction refluxed at 90° C. for 2 hours under a nitrogen atmosphere. The reaction was allowed to cool to room temp then partitioned between ethyl acetate (20 mL) and water (20 mL). The organics were dried over magnesium sulphate, filtered and concentrated in vacuo. The crude oil was dissolved in DCM and filtered to remove insoluble material. A brown solid precipitated from the filtrates and the filtrates were filtered again. The solid was analysed and found to be the desired material (1.9 g).

1. temperatureto cool to room temp
2. customthen partitioned between ethyl acetate (20 mL) and water (20 mL)
3. dry with materialThe organics were dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. dissolutionThe crude oil was dissolved in DCM
7. filtrationfiltered
8. customto remove insoluble material
9. customA brown solid precipitated from the filtrates
10. filtrationthe filtrates were filtered again