反应 #1885065

ord-cb1fc1fd7eca4765ae8b0bbc4d559e61

反应方程式

N
NH3
COc1cc2nc[nH]c(=O)c2cc1OC
6,7-dimethoxy-4(3H)-quinazolinone
COc1cccc2[nH]c(=O)nc(OC)c12
10
COc1cccc2[nH]c(=O)nc(OC)c12
dimethoxyquinazolinone
Br
HBr
O=c1[nH]cnc2cc(O)c(O)cc12
11
收率 84.0%
O=c1[nH]cnc2cc(O)c(O)cc12
6,7-dihydroxy-4(3H)-quinazolinone
收率 84.0%

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the solution was heated
  2. 2
    温度The reaction mixture was cooled to room temperature
  3. 3
    过滤the solids were filtered
  4. 4
    其他The solid obtained
  5. 5
    过滤the solution was filtered
  6. 6
    洗涤washed with water
  7. 7
    其他dried

实验过程

To 6,7-dimethoxy-4(3H)-quinazolinone, 10 (3.0 g, 14.5 mmol) was added 48% HBr (36 mL) and the solution was heated to reflux at 100° C. for 12 h. The reaction mixture was cooled to room temperature and the solids were filtered. The solid obtained was neutralized with aq. NH3 (pH=8) and the solution was filtered and washed with water and dried to give 6,7-dihydroxy-4(3H)-quinazolinone, 11 as a off-white crystalline solid (2.20 g, 84%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08343950B2uspto-grants-2013_01