Water → 2-Acetyl-6-(acetylaminomethyl)pyridine

HRID 1491814ノート

反応式

HRID 1491814 の反応式
[CH3:1][Mg]Br.[C:4]([NH:7][CH2:8][C:9]1[N:14]=[C:13]([C:15]#N)[CH:12]=[CH:11][CH:10]=1)(=[O:6])[CH3:5].[OH2:17]>O1CCCC1>[C:15]([C:13]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:8][NH:7][C:4](=[O:6])[CH3:5])[N:14]=1)(=[O:17])[CH3:1]

参加物

5

反応物 3

HCID 962WaterHCID 99897406-Acetylaminomethyl-2-pyridinecarbonitrileHCID 178418573HCID 178418573、化合物

生成物 1

HCID 103753152-Acetyl-6-(acetylaminomethyl)pyridine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

An ethereal solution of methyl magnesium bromide (3 mol/l) (17.6 ml) was added dropwise to a solution of 6-(acetylaminomethyl)-2-pyridinecarbonitrile (3.70 g) in tetrahydrofuran (60 ml) at 5 to 10° C. with stirring. After the mixture was stirred for two hours at the same temperature, cold water (15 ml) was dropped to the mixture under ice-cooling and evaporated in vacuo. The residue was mixed with water and extracted with a mixture of ethyl acetate and tetrahydrofuran. The extract was dried over magnesium sulfate and evaporated in vacuo. The residue was purified by silica gel column chromatography by eluting with a mixture of ethyl acetate and methanol (50:1) to give 2-acetyl-6-(acetylaminomethyl)pyridine (2.70 g).

後処理

  1. additionwas dropped to the mixture under ice-
  2. temperaturecooling
  3. customevaporated in vacuo
  4. additionThe residue was mixed with water
  5. extractionextracted with a mixture of ethyl acetate and tetrahydrofuran
  6. dry with materialThe extract was dried over magnesium sulfate
  7. customevaporated in vacuo
  8. customThe residue was purified by silica gel column chromatography
  9. washby eluting with a mixture of ethyl acetate and methanol (50:1)

出典と根拠

ORDレコード
ord-aed675aa9c9c499c8351a678b49a70f0
出典データセット
uspto-grants-1994_12
特許番号
US05371097

反応ノート

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