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Sulfuric Acid → HCID 22097097, 화합물

HRID 861493
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HRID 861493 반응식
N[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-:14])=[O:13])[N:8]([CH2:15][CH3:16])[C:7](=[O:17])[C:6](=[O:18])[NH:5]2.N([O-])=O.[Na+].S(=O)(=O)(O)O>C(O)(=O)C.C(O)C.[Cu-]=O>[CH2:15]([N:8]1[C:9]2[C:4](=[CH:3][CH:2]=[C:11]([N+:12]([O-:14])=[O:13])[CH:10]=2)[NH:5][C:6](=[O:18])[C:7]1=[O:17])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 1118Sulfuric AcidHCID 22097137HCID 22097137, 화합물HCID 23668193Sodium Nitrite

생성물 1

HCID 22097097HCID 22097097, 화합물수율 64%

시약·촉매·용매 3

HCID 178419072HCID 178419072, 화합물촉매HCID 176Acetic Acid용매
HCID 702
Ethanol
용매

실험 절차

14.2 g (57 mmol) of 6-amino-1-ethyl-7-nitro-2,3(1H,4H)-quinoxalinedione (Example 30a) were suspended in 340 ml of acetic acid. To this was added dropwise at 10°-20° C. a solution of 5.1 g (74 mmol) of sodium nitrite and 80 ml of concentrated sulfuric acid. The mixture was stirred for a further 30 minutes and then this solution was added dropwise to another suspension of 16.3 g (114 mmol) of copper(I) oxide in 140 ml ethanol. The mixture was stirred for a further 10 minutes and then poured into 11 of ice-water. After filtration, the filtrate was extracted with methylene chloride and the organic phase was dried and concentrated under reduced pressure to yield 8.5 g (64%) of the product. Melting point>300° C.

후처리

  1. stirringThe mixture was stirred for a further 10 minutes
  2. filtrationAfter filtration
  3. extractionthe filtrate was extracted with methylene chloride
  4. customthe organic phase was dried
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ed0709cb7cbc48cdb76b81d608cc1ecd
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05714489

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