Hydrogen Peroxide → 3-(Cyanomethyl)pyridin-1-ium-1-olate

HRID 1473139ノート

反応式

HRID 1473139 の反応式
[OH:1]O.[N:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][C:10]#[N:11])[CH:4]=1.O>C(O)(=O)C>[CH:7]1[CH:8]=[N+:3]([O-:1])[CH:4]=[C:5]([CH2:9][C:10]#[N:11])[CH:6]=1

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 809233-Pyridineacetonitrile

生成物 1

HCID 2431673-(Cyanomethyl)pyridin-1-ium-1-olate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
95 °C

実験手順

30% Hydrogen peroxide (12 mL) was added to a solution of 3-pyridylacetonitrile (7.50 g, 63.5 mmol) in acetic acid (40 mL) and the mixture heated at 95° C. for 20 hours. The reaction mixture was then cooled and stirred at room temperature for 72 hours. Water (35 mL) was then added and the solution concentrated under reduced pressure. Water (2×100 mL) was added to the residue and solution concentrated under reduced pressure. Residual water was removed azeotropically using toluene (2×100 mL) to yield the title compound (I115) (8.3 g, 97%) as a pale yellow solid which was used without further purification.

後処理

  1. temperatureThe reaction mixture was then cooled
  2. concentrationthe solution concentrated under reduced pressure
  3. additionWater (2×100 mL) was added to the residue and solution
  4. concentrationconcentrated under reduced pressure
  5. customResidual water was removed azeotropically using toluene (2×100 mL)

出典と根拠

ORDレコード
ord-15360e313ca94638b80559db319f6eb4
出典データセット
uspto-grants-2015_04
特許番号
US09012461B2

反応ノート

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