Water → 2-(2,4-Dichlorophenyl)-1-(3-pyridyl)-1-propanone

HRID 637297노트

반응식

HRID 637297 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[Cl:17])=[O:8])[CH:2]=1.[H-].[Na+].[CH3:20]I.O>CN(C)C=O>[Cl:17][C:11]1[CH:12]=[C:13]([Cl:16])[CH:14]=[CH:15][C:10]=1[CH:9]([CH3:20])[C:7]([C:3]1[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=1)=[O:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 136712392,4-Dichlorobenzyl 3-pyridyl ketone

생성물 1

HCID 140744312-(2,4-Dichlorophenyl)-1-(3-pyridyl)-1-propanone

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

28 g of 2,4-dichlorobenzyl 3-pyridyl ketone are dissolved in 800 ml of dimethylformamide and treated portionwise at 0° C. with 5.5 g of sodium hydride (50% dispersion in oil). After 2 hours at room temperature 14.9 g of methyl iodide are added and the mixture is stirred at room temperature for a further 3 hours. The mixture is then poured into water and extracted with diethyl ether. The organic phase is washed, dried over anhydrous sodium sulfate and subsequently concentrated. By chromatography on silica gel with n-hexane/ethyl acetate (1:2) there is obtained 2-(2,4-dichlorophenyl)-1-(3-pyridyl)-1-propanone as an oil.

후처리

  1. extractionextracted with diethyl ether
  2. washThe organic phase is washed
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationsubsequently concentrated

출처 및 근거

ORD 기록
ord-6a911e637a3b465ab76bd0d4a991664b
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04556661

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