2-Chloro-4-cyanopyridine → 2-Methoxyisonicotinonitrile

HRID 224870

反応式

HRID 224870 の反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][O-:11].[Na+]>CO.O1CCOCC1.CO>[CH3:10][O:11][C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1

参加物

5

反応物 2

HCID 5686382-Chloro-4-cyanopyridineHCID 10942334Sodium Methoxide

生成物 1

HCID 72048872-Methoxyisonicotinonitrile収率 110.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 21966525Dioxane Methanol溶媒

実験手順

2-Chloro-4-cyanopyridine (115.53 g) in methanol/dioxan (1:1, 850 ml) was added to a solution of sodium methoxide (prepared from 20.8 g sodium) in methanol (285 ml) and the mixture was boiled under reflux for 2.5 hours and was allowed to cool. The mixture was filtered and the volume of the filtrate was reduced by evaporation to 200 ml and water (400 ml) was added. The solid which precipitated out was filtered off to give 2-methoxy-4-cyanopyridine (57.2 g, 51%) m.p. 93°-95.5°.

後処理

  1. temperatureunder reflux for 2.5 hours
  2. temperatureto cool
  3. filtrationThe mixture was filtered
  4. customthe volume of the filtrate was reduced by evaporation to 200 ml and water (400 ml)
  5. additionwas added
  6. customThe solid which precipitated out
  7. filtrationwas filtered off

出典と根拠

ORDレコード
ord-fc4a7db47d314a38aaadf270ddc84200
出典データセット
uspto-grants-1980_11
特許番号
US04234588

関連ノート

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