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

HRID 1491814노트

반응식

HRID 1491814 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 99897406-Acetylaminomethyl-2-pyridinecarbonitrileHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 103753152-Acetyl-6-(acetylaminomethyl)pyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-aed675aa9c9c499c8351a678b49a70f0
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371097

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