1,3-dimethyl-1H-pyrazol-4-amine → 2-[[2-[(1,3-dimethylpyrazol-4-yl)amino]-5-(trifluoromethyl)-4-pyridyl]amino]-N-methoxy-benzamide

温度

150 °C

Palladium(II) acetate (7.79 mg, 0.03 mmol), (R)-(-)-1-[(S)-2-(Dicyclohexylphosphino)ferrocenyl]ethyldi-t-butylphosphine (19.46 mg, 0.03 mmol), Cesium carbonate (0.032 mL, 0.40 mmol), 1,3-dimethyl-1H-pyrazol-4-amine (38.6 mg, 0.35 mmol) and 2-(2-chloro-5-(trifluoromethyl)pyridin-4-ylamino)-N-methoxybenzamide (100 mg, 0.29 mmol) were suspended in DME (2.5 mL) and sealed into a microwave tube. The reaction was heated to 150 °C for 30 minutes in the microwave reactor and cooled to RT. The crude product was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH and pure fractions were evaporated to dryness to afford crude product as a orange gum. The sample was given to the purification group to be purified by preparative HPLC. Fractions containing the desired compound were evaporated to dryness to afford 2-(2-(1,3-dimethyl-1H-pyrazol-4-ylamino)-5-(trifluoromethyl)pyridin-4-ylamino)-N-methoxybenzamide (13.60 mg, 11.18 %) as a tan gum. The sample was not pure enough to register so will be re-made.

ORD记录

ord-f86ba050900b4317a90d58cd76e4f1c2

来源数据集

750 AstraZeneca ELN dataset

原始链接

查看来源