反应方程式
CNC(=O)c1ccccc1Nc1cc(Cl)ncc1C(F)(F)F.Cc1nn(C)cc1N>C1CCCC1.CC(=O)O.CC(=O)O.CC(C)(C)[O-].CC(C1CCCC1P(C1CCCCC1)C1CCCCC1)P(C(C)(C)C)C(C)(C)C.COCCOC.[Fe].[Na+].[Pd]>CNC(=O)c1ccccc1Nc1cc(Nc2cn(C)nc2C)ncc1C(F)(F)F参与物
反应物 2
产物 1
试剂、催化剂与溶剂 4
反应条件
- 温度
- 150 °C
实验过程
Palladium(II) acetate (8.17 mg, 0.04 mmol), (R)-(-)-1-[(S)-2-(Dicyclohexylphosphino)ferrocenyl]ethyldi-t-butylphosphine (20.40 mg, 0.04 mmol), Sodium tert-butoxide (0.052 mL, 0.42 mmol), 1,3-dimethyl-1H-pyrazol-4-amine (40.5 mg, 0.36 mmol) and 2-(2-chloro-5-(trifluoromethyl)pyridin-4-ylamino)-N-methylbenzamide (100 mg, 0.30 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 2-(2-(1,3-dimethyl-1H-pyrazol-4-ylamino)-5-(trifluoromethyl)pyridin-4-ylamino)-N-methylbenzamide (41.3 mg, 33.7 %) 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-methylbenzamide (41.3 mg, 33.7 %) as a yellow solid.
来源与证据
- ORD记录
- ord-2cb0b90157da471ebcc18c85cfe6adf7
- 来源数据集
- 750 AstraZeneca ELN dataset
- 原始链接
- 查看来源
关联笔记
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