Dimethylcarbamoyl Chloride → 5-Methoxy-6-methylpicolinonitrile

HRID 398253

반응식

HRID 398253 반응식
[CH3:1][O:2][C:3]1[C:4]([CH3:10])=[N+:5]([O-])[CH:6]=[CH:7][CH:8]=1.[C:11]([Si](C)(C)C)#[N:12].CN(C)C(Cl)=O>ClCCl>[C:11]([C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([CH3:10])[N:5]=1)#[N:12]

참가 물질

5

반응물 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 82115Trimethylsilyl cyanideHCID 122140163-Methoxy-2-methylpyridine 1-oxide

생성물 1

HCID 230024175-Methoxy-6-methylpicolinonitrile수율 11.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution obtained by dissolving 3-methoxy-2-methyl-pyridine-N-oxide (1.57 g, 11.3 mmol) in 30 ml of dichloromethane were added cyanotrimethylsilane (1.12 g, 11.3 mmol) and dimethylcarbamoyl chloride (1.21 g, 11.3 mmol), followed by stirring at room temperature for 9 days. The reaction solution was washed with 10% sodium carbonate aqueous solution and then with water. The organic layer was dried with sodium sulfate and concentrated to remove the solvent, by which 0.198 g (percent yield: 11.8%) of 2-cyano-5-methoxy-6-methylpyridine was obtained.

후처리

  1. customTo a solution obtained
  2. washThe reaction solution was washed with 10% sodium carbonate aqueous solution
  3. dry with materialThe organic layer was dried with sodium sulfate
  4. concentrationconcentrated
  5. customto remove the solvent

출처 및 근거

ORD 기록
ord-1d1b1b0466054e788516132c7d0acd6c
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610853B1

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