Dimethylformamide dimethyl acetal → 3-(Dimethylamino)-2-(furan-2-carbonyl)acrylonitrile

HRID 1111434노트

반응식

HRID 1111434 반응식
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[O:9]=[C:10]([C:14]1[O:15][CH:16]=[CH:17][CH:18]=1)[CH2:11][C:12]#[N:13]>>[CH3:6][N:4]([CH:3]=[C:11]([C:10](=[O:9])[C:14]1[O:15][CH:16]=[CH:17][CH:18]=1)[C:12]#[N:13])[CH3:5]

참가 물질

3

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 1416712-Furoylacetonitrile

생성물 1

HCID 515567863-(Dimethylamino)-2-(furan-2-carbonyl)acrylonitrile

실험 절차

A 50 ml portion of dimethylformamide dimethylacetal was added to 25 g of solid β-oxo-2-furanepropanenitrile. This exothermic reaction produced yellow crystals. After one hour the volatiles were removed under reduced pressure and the residue was dissolved in methylene chloride. This solution was passed through a short pad of hydrous magnesium silicate. The eluate was refluxed with the gradual addition of hexane to the point of turbidity. Cooling and filtration gave 35.2 g of the desired compound, mp 117°-125° C.

후처리

  1. customThis exothermic reaction
  2. customproduced yellow crystals
  3. customAfter one hour the volatiles were removed under reduced pressure
  4. dissolutionthe residue was dissolved in methylene chloride
  5. temperatureThe eluate was refluxed with the gradual addition of hexane to the point of turbidity
  6. temperatureCooling
  7. filtrationfiltration

출처 및 근거

ORD 기록
ord-d828157c2500496682d5c7adfb8946f8
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04980472

반응 노트

불러오는 중…