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

HRID 649650

반응식

HRID 649650 반응식
[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

참가 물질

3

반응물 2

HCID 944Nitric Acid2회HCID 757981,3-Benzodioxole, 5-nitro-

생성물 1

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

반응 조건

온도
-5 °C

실험 절차

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° C. 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° C.-100° C.). It can optionally be recrystallized from 96° strength ethanol.

후처리

  1. temperaturethe temperature being maintained at between 0° C. 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° C.-100° C.)
  5. customIt can optionally be recrystallized from 96° strength ethanol

출처 및 근거

ORD 기록
ord-ba65959a6a3e47ddaa5a7c2120f7f89b
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04740622

연결된 노트

불러오는 중…