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N,N,N',N'-Tetramethylethylenediamine → HCID 10445976, 화합물

HRID 1463426
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HRID 1463426 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([CH3:10])[C:3]=1[O:11][CH3:12].CN(C)CCN(C)C.C([Li])CCC.[CH:26](=[O:33])[C:27]1[CH:32]=[CH:31][CH:30]=[N:29][CH:28]=1>CCOCC.CCCCCC.O>[N:29]1[CH:30]=[CH:31][CH:32]=[C:27]([CH:26]([OH:33])[C:5]2[C:4]([CH3:10])=[C:3]([O:11][CH3:12])[C:2]([CH3:1])=[CH:7][C:6]=2[O:8][CH3:9])[CH:28]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 103713-PyridinecarboxaldehydeHCID 6433742,5-Dimethoxy-1,3-dimethylbenzeneHCID 178418339Butyllithium

생성물 1

HCID 10445976HCID 10445976, 화합물

시약·촉매·용매 3

HCID 962Water용매
HCID 3283
Diethyl Ether
용매
2회
HCID 8058Hexane용매

반응 조건

온도
-65 °C

실험 절차

3.0 g of 1,3-dimethyl-2,5-dimethoxybenzene and 3.1 g of tetramethylethylenediamine were dissolved in 30 ml of dry ether and 17 ml of a 1.6M solution of n-butyllithium in hexane was added dropwise thereto in a nitrogen atmosphere at room temperature. After 1 hour, the mixture was cooled to -65° C. and a solution of 2.9 g of nicotinaldehyde in 10 ml of ether was added thereto. After 30 minutes, the reaction was ceased by adding water and the reaction mixture was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate. After distilling off the solvent, 6.4 g of a crude product of the title compound was obtained.

후처리

  1. customat room temperature
  2. waitAfter 30 minutes
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. distillationAfter distilling off the solvent, 6.4 g of a crude product of the title compound
  6. customwas obtained

출처 및 근거

ORD 기록
ord-e6436a7a63314dceae549fd502051099
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05300518

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