反应详情

温度

95 °C

A solution of product from Step B (12.1 g), and 1-piperazinecarboxaldehyde (11 ml) in acetonitrile (150 ml) was heated at reflux for 16 hours. The acetonitrile was distilled at reduced pressure and the gummy residue treated with H2O (280 ml) and concentrated hydrochloric acid (70 ml) and heated at 95° C. for 1 hour. The solvent was distilled at reduced pressure, the residue treated with ammonium hydroxide, extracted with CH2Cl2 washed with water, brine and dried over K2CO3. The CH2Cl2 was distilled at reduced pressure and the residue chromatographed on silica gel (320 g) eluting with CHCl3 ·CH3OH (9:1). The pertinent fractions were combined and evaporated, the product dissolved in ethanol (60 ml), treated with 10N ethanolic HCl (10 ml) and ether (60 ml) to give 12.5 g of title compound which melted at 205°-207° C. after recrystallization from ethanol-ether.

1. temperatureat reflux for 16 hours
2. distillationThe acetonitrile was distilled at reduced pressure
3. additionthe gummy residue treated with H2O (280 ml) and concentrated hydrochloric acid (70 ml)
4. distillationThe solvent was distilled at reduced pressure
5. additionthe residue treated with ammonium hydroxide
6. extractionextracted with CH2Cl2
7. washwashed with water, brine
8. dry with materialdried over K2CO3
9. distillationThe CH2Cl2 was distilled at reduced pressure
10. customthe residue chromatographed on silica gel (320 g)
11. washeluting with CHCl3 ·CH3OH (9:1)
12. customevaporated
13. dissolutionthe product dissolved in ethanol (60 ml)
14. additiontreated with 10N ethanolic HCl (10 ml) and ether (60 ml)