1,2-Dichloroethane → ((2R)-2-(Cyclopentylmethyl)-3-{2-[2-ethyl-5-fluoro-6-(4-methyl-1-piperazinyl)-4-pyrimidinyl]hydrazino}-3-oxopropyl)[(phenylmethyl)oxy]formamide

関与物質

反応手順

A solution of (2R)-3-cyclopentyl-2-({formyl[(phenylmethyl)oxy]amino}methyl)propanoic acid (12.4 g, 40.6 mmol) in DMF (120 mL) was added to a mixture of 2-ethyl-5-fluoro-4-hydrazino-6-(4-methyl-1-piperazinyl)pyrimidine (9.6 g, 37.8 mmol), HOAt (5.66 g, 41.58 mmol), and EDC (7.97 g, 41.58 mmol). The resulting solution was treated with NMM (9.1 mL, 83.2 mmol) and stirred at room temperature for 3 h. After the reaction was complete, 200 mL of water was added and the solution was extracted three times with 200 mL of ether. The combined organic layers were washed with water (200 mL) and brine (100 mL), and then dried over anhydrous Na2SO4. Evaporation of the solvent provided a light yellow glassy solid as the pure product (17.1 g, 84%).

情報源と証拠