Ammonia → 2-Furanacetonitrile, alpha-amino-

HRID 586149

반응식

HRID 586149 반응식
[CH:1](=O)[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1.[C-:8]#[N:9].[Na+].[NH4+:11].[Cl-].N.CO.N>CO>[NH2:11][CH:1]([C:8]#[N:9])[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

실험 절차

Furfural (1.0 equiv) is mixed with NaCN (1.1 equiv) and NH4Cl (1.1 equiv) in 2 Molar NH3/MeOH (4 equiv NH3). The flask is fitted with a reflux condenser and mixture is refluxed. At the end of each of the first 3 h an additional equivalent of NH3 in MeOH is added. The reaction mixture is cooled and the excess solids are filtered away on a frit. The filtrate is concentrated by rotary evaporation and the residue is triturated with diethyl ether and the mixture is filtered again. The filtrate is concentrated on a rotovap. The product is purified, if necessary, by flash chromatography on silica gel with EtOAc/hexanes as an eluent to yield amino-cyano-(furan-2-yl)methane.

후처리

  1. customThe flask is fitted with a reflux condenser
  2. temperaturemixture is refluxed
  3. temperatureThe reaction mixture is cooled
  4. filtrationthe excess solids are filtered away on a frit
  5. concentrationThe filtrate is concentrated by rotary evaporation
  6. customthe residue is triturated with diethyl ether
  7. filtrationthe mixture is filtered again
  8. concentrationThe filtrate is concentrated on a rotovap
  9. customThe product is purified

출처 및 근거

ORD 기록
ord-b2d95a6cab124d4493b35da172c7f5e9
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936606B2

연결된 노트

불러오는 중…