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

HRID 2296611노트

반응식

HRID 2296611 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
0 °C

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-276c6523d4da4a44ad8656769ae49554
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06489322B1

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