反应详情

温度

120 °C

A solution of [3,5-bis(trifluoromethyl)benzyl]-(5-ethyl-pyrrolidin-3-yl)-[5-(1-methyl-1H-pyrazol-4-yl)-pyrimidin-2-yl]-amine (0.025 mmol, 12.5 mg), 2-chloro-oxazole-5-carboxylic acid ethyl ester (0.03 mmol, 5 mg) and N, N-diisopropylethylamine (0.03 mmol, 5 uL) in DMF (0.1 mL) is allowed to warm to 120° C. and stirred for 3 hours. The mixture is cooled to room temperature, then added with water. The mixture is extracted with CH2Cl2. The combined organic layer is dried over Na2SO4, filtrated, and concentrated under reduced pressure. The obtained residue is purified by silica gel column chromatography (eluent: n-hexane/EtOAc) to give 2-((2R,4S)-4-{(3,5-Bis-trifluoromethyl-benzyl)-[5-(1-methyl-1H-pyrazol-4-yl)-pyrimidin-2-yl]-amino}-2-ethyl-pyrrolidin-1-yl)-oxazole-4-carboxylic acid ethyl ester (7.4 mg, 46%); ESI-MS m/z: 638 [M+1]+, Retention time 2.20 min (condition A).

1. temperatureThe mixture is cooled to room temperature
2. extractionThe mixture is extracted with CH2Cl2
3. dry with materialThe combined organic layer is dried over Na2SO4
4. filtrationfiltrated
5. concentrationconcentrated under reduced pressure
6. customThe obtained residue is purified by silica gel column chromatography (eluent: n-hexane/EtOAc)