反应详情

温度

170 °C

A mixture of 1.0 g 1-chloro-4-(3-chloro-4-methoxybenzyl)amino-6-cyanophthalazine, 1.92 g (R)-(+)-3-hydroxypiperidine hydrochloride, 1.80 g diisopropyl ethylamine and 12 ml 1-methyl-2-pyrrolidone was stirred at 170° C. for 1 hr and 15 min. After cooling, ethyl acetate was added to the reaction solution which was then washed with water and brine. It was dried over anhydrous sodium sulfate, the solvent was evaporated, and the resulting residue was purified by silica gel column chromatography. The resulting free compound was suspended in acetic acid/ethanol/water, 1 N aqueous hydrochloric acid was added thereto, and it was dissolved by heating. After cooling, the resulting crystals were collected by filtration to give 860 mg of the title compound as a yellow powder.

1. temperatureAfter cooling
2. washwas then washed with water and brine
3. dry with materialIt was dried over anhydrous sodium sulfate
4. customthe solvent was evaporated
5. customthe resulting residue was purified by silica gel column chromatography
6. addition1 N aqueous hydrochloric acid was added
7. dissolutionit was dissolved
8. temperatureby heating
9. temperatureAfter cooling
10. filtrationthe resulting crystals were collected by filtration