Dimethylcarbamoyl Chloride → HCID 22494275, 화합물

HRID 1816592노트

반응식

HRID 1816592 반응식
[CH3:1][N:2](C)C(Cl)=O.C([O-])(=O)CCCCCCC/C=C\CCCCCCCC.[CH2:27]([O:29][C:30](=[O:43])[CH:31]([O:39][CH:40]([CH3:42])[CH3:41])[CH2:32][C:33]1[CH:38]=[CH:37][NH+:36]=[CH:35][CH:34]=1)[CH3:28].C[Si](C#N)(C)C.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[C:1]([C:37]1[CH:38]=[C:33]([CH2:32][CH:31]([O:39][CH:40]([CH3:42])[CH3:41])[C:30]([O:29][CH2:27][CH3:28])=[O:43])[CH:34]=[CH:35][N:36]=1)#[N:2]

참가 물질

6

반응물 4

HCID 6598Dimethylcarbamoyl ChlorideHCID 11430Potassium CarbonateHCID 82115Trimethylsilyl cyanideHCID 69801129HCID 69801129, 화합물

생성물 1

HCID 22494275HCID 22494275, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2.3 mL dimethyl carbamyl chloride was added dropwise over 40 minutes into a solution of 6.40 g crude 4-(3-ethoxy-2-isopropoxy-3-oxopropyl)-1-pyridinium oleate and 3.3 mL trimethylsilyl cyanide in dichloromethane (60 mL), followed by stirring for 11.5 hours. 10% aqueous potassium carbonate was added to the reaction solution, followed by stirring at room temperature for 30 minutes. The organic layer was dried over anhydrous sodium sulfate and concentrated. The residue was purified by silica gel flash column chromatography, to give 3.87 g of ethyl 3-(2-cyano-4-pyridyl)-2-isopropoxypropanoate as a pale yellow oil.

후처리

  1. stirringby stirring at room temperature for 30 minutes
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by silica gel flash column chromatography

출처 및 근거

ORD 기록
ord-e7fbc273b335441fa0e87c8d899086ff
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06884821B1

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