Nitric Acid → 5,6-Dinitro-1,3-benzodioxole

HRID 579687

反応式

HRID 579687 の反応式
[CH2:1]1[O:9][C:8]2[C:3](=[CH:4][CH:5]=[C:6]([N+:10]([O-:12])=[O:11])[CH:7]=2)[O:2]1.[N+:13]([O-])([OH:15])=[O:14]>>[CH2:1]1[O:2][C:3]2[C:8](=[CH:7][C:6]([N+:10]([O-:12])=[O:11])=[C:5]([N+:13]([O-:15])=[O:14])[CH:4]=2)[O:9]1

参加物

3

反応物 2

HCID 944Nitric Acid2 回HCID 757981,3-Benzodioxole, 5-nitro-

生成物 1

HCID 6113255,6-Dinitro-1,3-benzodioxole

反応条件

温度
-5 °C

実験手順

0.103 mol (17.2 g) of 4,5-methylenedioxy-1-nitrobenzene is added in small portions in the course of 15 minutes to a mixture, cooled to -5° C., consisting of 125 ml of nitric acid (d=1.50) and 125 ml of nitric acid (d=1.40), the temperature being maintained at between 0° and 5° C. 1 hour after the addition is complete, the reaction mixture is poured onto 1 kg of ice. The expected product precipitates. After being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98°-100° C.). It can optionally be recrystallized from 96° strength ethanol.

後処理

  1. temperaturethe temperature being maintained at between 0° and 5° C
  2. addition1 hour after the addition
  3. customThe expected product precipitates
  4. dry with materialAfter being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98°-100° C.)
  5. customIt can optionally be recrystallized from 96° strength ethanol

出典と根拠

ORDレコード
ord-7a1e47a7683e4485b828e5fb555ebd67
出典データセット
uspto-grants-1988_06
特許番号
US04749379

関連ノート

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