反応 #2383793

ord-276c6523d4da4a44ad8656769ae49554

反応方程式

O=C1NCCOc2ccccc21
2,3,4,5-tetrahydro-1,4-benzoxazepin-5-one
O=[N+]([O-])[O-].[K+]
potassium nitrate
O=C1NCCOc2ccc([N+](=O)[O-])cc21
title compound
収率 22.2%
O=C1NCCOc2ccc([N+](=O)[O-])cc21
7-Nitro-2,3,4,5-tetrahydro-1,4-benzoxazepin-5-one
収率 22.2%

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITfor 4 h at room temperature
  2. 2
    ろ過the solids were collected by filtration
  3. 3
    温度cooled

実験手順

To 2,3,4,5-tetrahydro-1,4-benzoxazepin-5-one (30.34 g, 190 mmol) in conc. sulfuric acid (600 ml) at 0° C. was added potassium nitrate (20.82 g, 206 mmol) portionwise. The mixture was stirred for 20 minutes at 0° C. and then for 4 h at room temperature. The mixture was poured onto ice (21) and the solids were collected by filtration. The solids were taken up in hot ethyl acetate and then cooled to yield the title compound (8.79 g, 22%), MS m/z 209 [M+H]+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06489322B1uspto-grants-2002_12