Potassium Nitrate → 7-nitro-3,4-dihydro-1,4-benzoxazepin-5(2H)-one

HRID 2296611ノート

反応式

HRID 2296611 の反応式
[O:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5](=[O:12])[NH:4][CH2:3][CH2:2]1.[N+:13]([O-])([O-:15])=[O:14].[K+]>S(=O)(=O)(O)O>[N+:13]([C:10]1[CH:9]=[CH:8][C:7]2[O:1][CH2:2][CH2:3][NH:4][C:5](=[O:12])[C:6]=2[CH:11]=1)([O-:15])=[O:14]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 3406292,3,4,5-Tetrahydro-1,4-benzoxazepin-5-one

生成物 1

HCID 183874717-nitro-3,4-dihydro-1,4-benzoxazepin-5(2H)-one収率 22.2%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
0 °C

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]+.

後処理

  1. waitfor 4 h at room temperature
  2. filtrationthe solids were collected by filtration
  3. temperaturecooled

出典と根拠

ORDレコード
ord-276c6523d4da4a44ad8656769ae49554
出典データセット
uspto-grants-2002_12
特許番号
US06489322B1

反応ノート

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