HRID2396466

反应详情

EQUATION

反应方程式

HRID 2396466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

3-Methoxy-2,5-dioxo-2,5-dihydro-1H-benz[b]azepine (1.0 g) was treated with diethanolamine (10 mL), and the mixture was heated to 140° C. for 2 hours. The mixture was diluted with water and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried and evaporated. The solid was recrystalized from ethanol to give the title compound (53 mg); mp 204°-205° C.; NMR: 5.90 (s,1); MS: m/z=277(+1). Analysis for C14H16NO4 : Calculated: C, 60.80; H, 5.84; N, 10.14; Found: C, 61.29; H, 5.29; N, 11.74.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe combined organic extracts were washed with brine
  3. customdried
  4. customevaporated
  5. customThe solid was recrystalized from ethanol