Dimethylformamide → (9-Ethyl-9H-carbazol-3-yl)ethene-1,1,2-tricarbonitrile

HRID 435557

반응식

HRID 435557 반응식
[CH2:1]([N:3]1[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH3:2].CN(C)C=O.[C:21]([C:23]([C:29]#[N:30])=[C:24](C#N)[C:25]#[N:26])#[N:22]>O>[CH2:1]([N:3]1[C:15]2[CH:14]=[CH:13][C:12]([C:24]([C:25]#[N:26])=[C:23]([C:29]#[N:30])[C:21]#[N:22])=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH3:2]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 6836N-ethyl carbazoleHCID 12635Tetracyanoethylene

생성물 1

HCID 18627189(9-Ethyl-9H-carbazol-3-yl)ethene-1,1,2-tricarbonitrile

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

About 1 gram (5.24 × 10-3 3 moles) N-ethyl carbazole and 20 milliliters of dimethylformamide are placed in a 50 milliliter one neck flask equipped with a magnetic stirring bar and a nitrogen inlet tube. The flask is purged of air with nitrogen, the contents of the flask agitated and about 0.67 grams (5.24 × 10-3 moles) of tetracyanoethylene introduced into the flask. Upon the admixture of these materials the contents of the flask turns deep blue. This mixture is heated to 100° C for 20 hours, the contents of the flask poured into 60 milliliters of water at room temperature and the redish brown crystals thereby precipitated isolated from the solution by filtration and washed with ethanol. Yield: 1.13 grams brick red crystals m. p. 239°-241° C. Analysis: calculated, carbon 77, hydrogen 4.08, nitrogen 18.92; actual, carbon 77.24, hydrogen 4.07, nitrogen 18.78.

후처리

  1. customequipped with a magnetic stirring bar and a nitrogen inlet tube
  2. customThe flask is purged of air with nitrogen
  3. customthe redish brown crystals thereby precipitated
  4. customisolated from the solution by filtration
  5. washwashed with ethanol

출처 및 근거

ORD 기록
ord-68f4db311fb54625a753fb7fe583c265
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04006017

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