Hydrogen Peroxide → diethyl pyridine-2,3-dicarboxylate-N-oxide

HRID 1741618ノート

反応式

HRID 1741618 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:2]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13].S(=O)(=O)(O)[OH:18].OO>C(O)(=O)C>[N+:1]1([O-:18])[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[C:2]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13]

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 108895172,3-Diethyl 2,3-pyridinedicarboxylate

生成物 1

HCID 21847052diethyl pyridine-2,3-dicarboxylate-N-oxide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 99 g of diethyl pyridine-2,3-dicarboxylate, 7.2 mL of concentrated sulfuric acid, 85 mL of 30% hydrogen peroxide and 256 mL acetic acid is stirred and heated at 85° for 4 hours. The reaction is concentrated in vacuo, and the residue is dissolved in methylene chloride, and washed with water, then saturated sodium bicarbonate. After drying, the organic phase is concentrated in vacuo to afford 79 g of the desired product, mp 80°-85°. A portion recrystallized from carbon tetrachloride-pentane has mp 87°-88°.

後処理

  1. temperatureheated at 85° for 4 hours
  2. concentrationThe reaction is concentrated in vacuo
  3. dissolutionthe residue is dissolved in methylene chloride
  4. washwashed with water
  5. customAfter drying
  6. concentrationthe organic phase is concentrated in vacuo

出典と根拠

ORDレコード
ord-0f083197b39c4f41b4d58c3f08ed1bd2
出典データセット
uspto-grants-1994_08
特許番号
US05334576

反応ノート

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