反应详情

温度

150 °C

A mixture of 1-(5-fluoropyrimidin-2-yl)ethanamine hydrochloride (252 mg, 1.42 mmol), 2-chloro-7-cyclopropyl-N-(1-methyl-1H-imidazol-4-yl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine (205 mg, 0.71 mmol), palladium(II) acetate (15.94 mg, 0.07 mmol) and palladium(II) acetate (15.94 mg, 0.07 mmol) (R)-(-)-1-[(S)-2-(DICYCLOHEXYLPHOSPHINO)FERROCENYL]ETHYLDI-T-BUTYLPHOSPHINE (62.1 mg, 0.11 mmol) and CS2CO3 (1619 mg, 4.97 mmol) in 1,4-dioxane (4733 µl) was heatd to 150 oC for 20 min with well-stirring. Reaction was diluted with DCM/MeOh (10%) the organic layer was washed with water. And concntraction provided product. Reaction is clean and 70% contaminated with hydroxy product (P3). Reaction was purified on gilsen (5 to 45%) provide product 40 mg. Compound was submitted to chiral purification. Chiral sepreation: En02021-65-2 (P2, E1) : EN02021-65-3 (P3, E2) = 4:96 There is no racemization observed in reaction.