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Sulfuric Acid → HCID 22097097、化合物

HRID 861493
ノート
印刷プレビュー

反応式

HRID 861493 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 1118Sulfuric AcidHCID 22097137HCID 22097137、化合物HCID 23668193Sodium Nitrite

生成物 1

HCID 22097097HCID 22097097、化合物収率 64%

試薬・触媒・溶媒 3

HCID 178419072HCID 178419072、化合物触媒HCID 176Acetic Acid溶媒
HCID 702
Ethanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ed0709cb7cbc48cdb76b81d608cc1ecd
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05714489

反応ノート

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