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Nitric Acid → Y 9000

HRID 1579400
ノート
印刷プレビュー

反応式

HRID 1579400 の反応式
[N+]([O-])(O)=O.[Mn]([O-])(=O)(=O)=O.[K+].[O-2:11].[Mg+2].[CH2:13]([C:15]1[CH:16]=[CH:17][C:18]2[O:27][C:22]3=[N:23][CH:24]=[CH:25][CH:26]=[C:21]3[C:20](=[O:28])[C:19]=2[CH:29]=1)[CH3:14]>O>[C:13]([C:15]1[CH:16]=[CH:17][C:18]2[O:27][C:22]3=[N:23][CH:24]=[CH:25][CH:26]=[C:21]3[C:20](=[O:28])[C:19]=2[CH:29]=1)(=[O:11])[CH3:14]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 944Nitric AcidHCID 516875Potassium PermanganateHCID 6850729Magnesium monoxideHCID 12689276HCID 12689276、化合物

生成物 1

HCID 198324Y 9000収率 67%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

7.6 ml of nitric acid (specific gravity 1.38) and 7.9 g of potassium permanganate are added to a suspension of 2 g of magnesium oxide in 50 ml of water, and the mixture is heated to 60°C. To the mixture is added 4.5 g of 7-ethyl-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine over a period of 30 minutes with stirring, keeping the temperature at 60°-70°C. After the addition the mixture is stirred at 60°-70°C for 4.5 hours. After cooling, the reaction mixture is filtered under reduced pressure, and the residue containing manganese dioxide is extracted several times with chloroform. The chloroform layer is washed with water, dried, and the chloroform is distilled off. The residue is recrystallized from toluene to give 3.2 g of 7-acetyl-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine melting at 195°-196°C.

後処理

  1. customat 60°-70°C
  2. additionAfter the addition the mixture
  3. stirringis stirred at 60°-70°C for 4.5 hours
  4. temperatureAfter cooling
  5. filtrationthe reaction mixture is filtered under reduced pressure
  6. additionthe residue containing manganese dioxide
  7. extractionis extracted several times with chloroform
  8. washThe chloroform layer is washed with water
  9. customdried
  10. distillationthe chloroform is distilled off
  11. customThe residue is recrystallized from toluene

出典と根拠

ORDレコード
ord-89d1f736538b45978b4be8a93a2bd148
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03931199

反応ノート

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