Acetic Acid → 3-(Cyanomethyl)pyridin-1-ium-1-olate

HRID 428550ノート

反応式

HRID 428550 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]#[N:9])[CH:2]=1.CC(O)=[O:12].OO>O>[CH:5]1[CH:6]=[N+:1]([O-:12])[CH:2]=[C:3]([CH2:7][C:8]#[N:9])[CH:4]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 809233-Pyridineacetonitrile

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 3-pyridylacetonitrile (11 g, 93.1 mmol), HOAc (55 mL), and 30% H2O2 (17 mL) was heated at 95° C. overnight, and at room temperature for 72 hours. H2O (50 mL) was added to the reaction mixture and the resulting solution was concentrated. This was repeated with additional H2O (100 mL). Toluene (2×100 mL) was used to remove residual H2O, and the resulting white solid was dried under vacuum overnight affording a waxy white solid: mp 120-125° C.; MS(+)APCI m/z 135 [M+H]+.

後処理

  1. concentrationthe resulting solution was concentrated
  2. customto remove residual H2O
  3. customthe resulting white solid was dried under vacuum overnight
  4. customaffording a waxy white solid

出典と根拠

ORDレコード
ord-0cff787d32e24df79972a709b0996a6c
出典データセット
uspto-grants-2001_11
特許番号
US06313126B1

反応ノート

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