HRID128023

反应详情

EQUATION

反应方程式

HRID 128023 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooled
  2. customThe solid portion of the reaction mixture was collected on
  3. filtrationa filter
  4. washwashed with methylene chloride