HRID2255909

反应详情

EQUATION

反应方程式

HRID 2255909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-methoxy-2,5-dioxo-2,5-dihydro-1H-benz[b]azepine (1.0 g) in methanol (20 mL) was added ethanolamine (0.36 g). The mixture was heated to reflux until a precipitate formed. The reaction mixture was cooled to room temperature, filtered, and the resulting solid was recrystallized from ethanol to give the title compound (0.72 g); mp 207° C.; NMR: 5.91 (s,1); MS(EI): m/z=232(M). Analysis for C12H12N2O3.0.2 H2O: Calculated: C, 61.11; H, 5.30; N, 11.88; Found: C, 61.13; H, 5.20; N, 11.72.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux until a precipitate
  3. customformed
  4. filtrationfiltered
  5. customthe resulting solid was recrystallized from ethanol