HRID235151

反应详情

EQUATION

反应方程式

HRID 235151 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product of Example 11 (7-benzamido-1-(1-piperazinyl)-naphthalene, (0.063 g, 0.19 mmol) was combined with hydrochloric acid in ethanol (4 mL) and refluxed 16 hours. The reaction was concentrated at reduced pressure and the residue was neutralized with 4 N sodium hydroxide and extracted with methylene chloride. The organic phase was washed with brine, dried and concentrated to a tan solid (0.041 g). The solid was recrystallized from ethyl acetate/hexane to give 0.020 g (47%) of the title compound as light tan crystals. mp 184°-186° C. HRMS m/e calculated for C14H17N3 : 227.1419. Observed m/e 227.1405.

WORKUP

后处理

  1. temperaturerefluxed 16 hours
  2. concentrationThe reaction was concentrated at reduced pressure
  3. extractionextracted with methylene chloride
  4. washThe organic phase was washed with brine
  5. customdried
  6. concentrationconcentrated to a tan solid (0.041 g)
  7. customThe solid was recrystallized from ethyl acetate/hexane