反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Prepared from 2-amino-6(5H)-phenanthridinone 3 and succinic anhydride. To a solution of 2-amino-6(5H)-phenanthridinone (150 mg, 0.71 mmol) in dioxane (30 mL) was added a solution of succinic anhydride (87 mg, 1.1 mmol) in dioxane (5 mL) over 5 minutes. The mixture was stirred for 16 hours and a yellowish precipitation was formed. Purification of the precipitation by crystallization in dioxane gave a light white solid (92% yield), mp 224-228° C. 1H-NMR (400 MHz DMSO-d6), 11.7 (s, 1H), 10.1 (s, 1H), 8.67 (s, 1H), 8.33 (d, J=7.8 Hz, 1H), 8.24 (d, J=8.2 Hz, 1H), 7.87 (t, J=7.0 Hz, 1H), 7.66 (t, J=7.44 Hz, 1H), 7.60 (t, J=8.7 Hz, 1H),7.30 (d, J=8.7 Hz, 1H), 2.60 ((d, J=5.4 Hz, 2H), 2.56 (d, J=5.4 Hz, 2H). Anal. (C17H24N2O4 .0.1 H2O), C H N.
WORKUP
后处理
- customa yellowish precipitation
- customwas formed
- customPurification of the precipitation
- customby crystallization in dioxane