反应详情

温度

100 °C

In a high-pressure vessel was placed (S)-4-(2-chloro-8-iodo-9-methyl-9H-purin-6-yl)-3-methylmorpholine (78.2 mg, 0.20 mmol), cyclopropylboronic acid (25.8 mg, 0.30 mmol, 1.5 eq.), potassium phosphate (127.4 mg, 0.60 mmol, 3.0 eq.), [1,1′-bis-(diphenylphosphino)ferrocene]dichloropalladium (II), complexed with dichloromethane (1:1) (4.9 mg, 0.006 mmol, 0.03 eq.), and 1,4-dioxane (1.0 mL). The reaction mixture was degassed for 15 minutes. The vessel tube was sealed tightly, and the reaction mixture was stirred at 100° C. After 18 h the reaction was cooled to RT and diluted with ethyl acetate. The organic layer was washed with water and brine, then dried (Na2SO4), filtered and evaporated in vacuo. The resultant residue was purified by column chromotagraphy (Si-PPC, gradient 0 to 80% ethyl acetate in hexane) to give the desired compound as a foam (43.7 mg, 71%). TLC (40% ethyl acetate/hexane), Rf=0.41; LC-MS m/z (method B2)=308 [M+H]+, RT=1.94 min.

1. customIn a high-pressure vessel was placed
2. customThe reaction mixture was degassed for 15 minutes
3. customThe vessel tube was sealed tightly
4. temperatureAfter 18 h the reaction was cooled to RT
5. additiondiluted with ethyl acetate
6. washThe organic layer was washed with water and brine
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customevaporated in vacuo
10. customThe resultant residue was purified by column chromotagraphy (Si-PPC, gradient 0 to 80% ethyl acetate in hexane)