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 n-butylacetate (92 ml; Example 8) was added ethanol (235.3 ml) followed by n-butylacetate (117.7 ml) and the solution was heated to 60° C. Seed (0.1 g) was added to the hot solution followed by a solution of hydrochloric acid in isopropanol (13.44 ml, 4.68M, 62.9 mol) and the solution cooled to −10° C. over 10 hrs. The crystals were filtered and washed twice with ethanol (20 ml). After drying at 40° C. under vacuum gave 21.46 g, 79% yield of (5-Cyano-2-nitro-phenyl)-(5-morpholin-4-ylmethyl-pyridin-2-yl)-acetic acid ethyl ester hydrochloride salt as red wine crystals. Characterisation data were in accordance with example 7.

1. additionSeed (0.1 g) was added to the hot solution
2. temperaturethe solution cooled to −10° C. over 10 hrs
3. filtrationThe crystals were filtered
4. washwashed twice with ethanol (20 ml)
5. customAfter drying at 40° C. under vacuum