Hydrogen Peroxide → HCID 10016333, 화합물

HRID 465333노트

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HRID 465333 반응식
[N+:1](C1C=C2C(=CC=1)N1N=NN=C1C=N2)([O-:3])=[O:2].OO.[N+:19]([C:22]1[CH:23]=[C:24]2[C:29](=[CH:30][CH:31]=1)[N:28]1[N:32]=[N:33][N:34]=[C:27]1[C:26](=[O:35])[NH:25]2)([O-:21])=[O:20].OS(O)(=O)=O.[N+]([O-])([O-])=O.[K+]>O.CC(O)=O>[N+:19]([C:22]1[CH:23]=[C:24]2[C:29](=[CH:30][C:31]=1[N+:1]([O-:3])=[O:2])[N:28]1[N:32]=[N:33][N:34]=[C:27]1[C:26](=[O:35])[NH:25]2)([O-:21])=[O:20]

참가 물질

8

반응물 5

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 24434Potassium NitrateHCID 100598007-nitrotetrazolo[1,5-a]quinoxalin-4(5H)-oneHCID 10420849HCID 10420849, 화합물

생성물 1

HCID 10016333HCID 10016333, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

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온도
85 °C

실험 절차

The nitrotetrazoloquinoxaline (23) (1.84 g, 8.51 mmol) was added to a mixture of 15 ml of glacial AcOH and 20 ml of 30% H2O2 and heated at 85° C. in an oil bath for 16 hours. Upon cooling, the mixture was diluted with H2O (50 ml) and the precipitate collected by filtration. Recrystallization from 40 ml of 50% aq. DMF gave 1.29 g of yellow flocculant needles comprising 7-nitrotetrazolo[1,5-a]quinoxalin-4(5H)-one (24). This nitrotetrazoloquinoxalinone (3.00 g, 12.9 mmol) was added to conc. H2SO4 (40 ml) and treated with KNO3 (1.43 g, 14.1 mmol) with warming to 50° C. under N2. The mixture was poured onto 600 ml of ice-H2O, and a light yellow solid collected by filtration and washed with H2O, yielding 7,8-dinitrotetrazolo[1,5-a]quinoxalin-4(5H)-one (25).

후처리

  1. temperatureUpon cooling
  2. filtrationthe precipitate collected by filtration
  3. customRecrystallization from 40 ml of 50% aq. DMF
  4. customgave 1.29 g of yellow flocculant needles
  5. temperaturewith warming to 50° C. under N2
  6. filtrationa light yellow solid collected by filtration
  7. washwashed with H2O

출처 및 근거

ORD 기록
ord-3887cf5c3820452a80fa71767d5137f5
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05153196

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