HRID128023
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 100 g (0.43 mole) of 2-amino-5-chlorobenzophenone and 40 g (0.7 mole) of methyl isocyanate in 300 ml of methylene chloride was refluxed for two days and then cooled. The solid portion of the reaction mixture was collected on a filter and washed with methylene chloride to give 119.8 g (96% yield) of 6-chloro-3,4-dihydro-4-hydroxy-3-methyl-4-phenyl-2(1H)-quinazolinone as a white crystalline powder: mp 296°-298° (dec); 1H nmr (DMSO-d6), δ 2.66 ppm (s, 3H), 6.8-7.6 ppm (m, 8H) and 10.0 ppm (s, NH); 13C nmr (DMSO-d6) δ 86.6 ppm (for COH) and 151.4 ppm (for NHCO).
WORKUP
后处理
- temperaturecooled
- customThe solid portion of the reaction mixture was collected on
- filtrationa filter
- washwashed with methylene chloride