Dimethyl Sulfate → 6-(2-p-Tolyl-vinyl)-pyridine-2-carbonitrile

HRID 965853

反応式

HRID 965853 の反応式
[C:1]1([CH3:16])[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N+:10]=2[O-])=[CH:3][CH:2]=1.COS(OC)(=O)=O.[C-:24]#[N:25].[Na+]>C(O)(C)C>[C:1]1([CH3:16])[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][C:9]2[N:10]=[C:11]([C:24]#[N:25])[CH:12]=[CH:13][CH:14]=2)=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 8929Sodium CyanideHCID 695921292-(2-p-Tolyl-vinyl)-pyridine 1-oxide

生成物 1

HCID 695920426-(2-p-Tolyl-vinyl)-pyridine-2-carbonitrile

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

In a variation to the procedure referred to in example 1, 2-(2-p-tolyl-vinyl)-pyridine 1-oxide (9.8 g, 46 mmol) was reacted first with dimethylsulfate ( 5.8 g, 46 mmol) and then with NaCN (2.74 g, 56 mmol). After extraction and crystallization 6-(2-p-tolyl-vinyl)-pyridine-2-carbonitrile (5.8 g, 57%) was obtained as a yellow crystalline material. Mp. 137-138° C. (isopropanol), MS: m/e=220 (M+)

後処理

  1. extractionAfter extraction
  2. customcrystallization 6-(2-p-tolyl-vinyl)-pyridine-2-carbonitrile (5.8 g, 57%)
  3. customwas obtained as a yellow crystalline material

出典と根拠

ORDレコード
ord-4f80f94ca7fb497abb25fde0d2a3ffae
出典データセット
uspto-grants-2005_10
特許番号
US06951875B2

関連ノート

読み込み中…