反应详情

温度

150 °C

To a solution of (2R,4S)-4-{(3,5-bis-trifluoromethyl-benzyl)-[5-(1-methyl-1H-pyrazol-4-yl)-pyrimidin-2-yl]-amino}-2-ethyl-pyrrolidine-1-carboxylic acid 4-nitro-phenyl ester (0.03 mmol, 20 mg) in 1 mL of DMF are added trans-4-(aminomethyl)cyclohexanecarboxylic acid methyl ester hydrochloride (0.04 mmol, 8 mg) and triethylamine (0.07 mmol, 0.01 mL). The mixture is stirred under microwave irradiation (150° C., 5 bar), then cooled to room temperature. The mixture is poured into a saturated aqueous ammonium chloride and extracted with dichloromethane. The combined organic phases is washed by water and brine, dried over anhydrous Na2SO4 and evaporated. The obtained residue is purified by column chromatography on silica gel (eluent: n-hexane-ethyl acetate) to obtain 12.3 mg (59%) of (2R,4S)-4-{(3,5-Bis-trifluoromethyl-benzyl)-[5-(1-methyl-1H-pyrazol-4-yl)-pyrimidin-2-yl]-amino}-2-ethyl-pyrrolidine-1-carboxylic acid dimethylamide as colorless oil. ESI-MS m/z: 570 [M+1]+, Retention time 4.05 min (condition B).

1. temperaturecooled to room temperature
2. extractionextracted with dichloromethane
3. washThe combined organic phases is washed by water and brine
4. dry with materialdried over anhydrous Na2SO4
5. customevaporated
6. customThe obtained residue is purified by column chromatography on silica gel (eluent: n-hexane-ethyl acetate)