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
PROCEDURE
实验过程
A solution of 109 mg of N-(6-nitro-2,4-dioxo-7-trifluoromethyl-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide in 3 ml of ethanol and 3 ml of acetic acid is hydrogenated in the presence of 30 mg of 10% palladium on carbon. After disappearance of the starting material followed by TLC the reaction mixture is diluted with ethanol and acetic acid and slightly warmed up. The catalyst is filtered off and the filtrate concentrated to dryness. Trituration of the residue with ethyl acetate gives 61 mg (61%) of N-(6-amino-2,4-dioxo-7-trifluoromethyl-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide as a yellow powder, m.p. 240° C. (decomp.). 1H-NMR (DMSO-d6, 400 MHz): 3.12 (s, 3H); 5.66 (s, 2H); 7.24 (s, 1H); 7.46 (s, 1H); 10.3 (br s, 1H); 11.4 (br s, 1H).
WORKUP
后处理
- temperatureslightly warmed up
- filtrationThe catalyst is filtered off
- concentrationthe filtrate concentrated to dryness