反应详情

温度

60 °C

To the (5-Cyano-2-nitro-phenyl)-(5-morpholin-4-ylmethyl-pyridin-2-yl)-acetic acid ethyl ester solution in toluene (196 ml; Example 7) was added ethanol (394 ml) and the solution is heated to 60° C. A solution of hydrochloric acid in isopropanol (26.8 ml, 4.87M, 103.3 mol) was then added followed by addition of seeds (317 mg) and the solution cooled to −10° C. over 10 hrs. The crystals were filtered and washed three times with ethanol (63 ml). After drying at 40° C. under vacuum gave 48.62 g, 87% yield of (5-Cyano-2-nitro-phenyl)-(5-morpholin-4-ylmethyl-pyridin-2-yl)-acetic acid ethyl ester hydrochloride salt as red wine crystals.

1. additionfollowed by addition of seeds (317 mg)
2. temperaturethe solution cooled to −10° C. over 10 hrs
3. filtrationThe crystals were filtered
4. washwashed three times with ethanol (63 ml)
5. customAfter drying at 40° C. under vacuum