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

HRID 1473139노트

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HRID 1473139 반응식
[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

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 809233-Pyridineacetonitrile

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
95 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-15360e313ca94638b80559db319f6eb4
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09012461B2

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