HRID2396466
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionextracted with ethyl acetate
- washThe combined organic extracts were washed with brine
- customdried
- customevaporated
- customThe solid was recrystalized from ethanol