反应 #657349

ord-a369aaa1b46948c3b632be5438e216a0

反应方程式

COc1ccc(N)c(C(=O)O)c1
5-methoxyanthranilic acid
CC(=O)OC(C)=O
acetic anhydride
COc1ccc2nc(C)oc(=O)c2c1
title compound
收率 77.0%
COc1ccc2nc(C)oc(=O)c2c1
2-methyl-6-(methyloxy)-4H-3,1-benzoxazin-4-one
收率 77.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度before being cooled
  2. 2
    浓缩concentrated under reduced pressure
  3. 3
    浓缩The crude residue was then concentrated twice in the presence of toluene
  4. 4
    过滤before being filtered
  5. 5
    洗涤washed with ether

实验过程

A solution of 5-methoxyanthranilic acid (7.8 g, 46.5 mmol) was refluxed in acetic anhydride (60 mL) for 2 h15 before being cooled and concentrated under reduced pressure. The crude residue was then concentrated twice in the presence of toluene before being filtered and washed with ether to yield to the title compound (6.8 g, 77% yield) as a beige solid; LC/MS: m/z 192 [M+H]+, Rt 1.69 min.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09023842B2uspto-grants-2015_05