Formic Acid → 5-Chloro-2-(2,2,2-trifluoroethoxy)benzaldehyde

HRID 1600200노트

반응식

HRID 1600200 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:10][CH2:11][C:12]([F:15])([F:14])[F:13])=[C:6]([CH:9]=1)[C:7]#N.C(O)=[O:17]>[Ni]>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:10][CH2:11][C:12]([F:15])([F:14])[F:13])=[C:6]([CH:9]=1)[CH:7]=[O:17]

참가 물질

4

반응물 2

HCID 284Formic AcidHCID 190751615-Chloro-2-(2,2,2-trifluoroethoxy)benzonitrile

생성물 1

HCID 47709505-Chloro-2-(2,2,2-trifluoroethoxy)benzaldehyde

시약·촉매·용매 1

HCID 935Nickel촉매

실험 절차

Under a nitrogen atmosphere, in a round-bottom flask equipped with a refluxcondenser were placed 400 mg (1.7 mmol) of the above nitrile and 10 ml of formic acid. To the system were added ca. 500 mg of Raney nickel and the mixture was heated at reflux for 6 hours and stirred at room temperature overnight. The mixture was filtered through a pad of a diatomaceous earth,and the pad was rinsed with water and CHCl3. The layers were separatedand the aqueous phase was extracted with three portions of CHCl3. The combined organic fractions were dried and concentrated to obtain 270 mg ofthe title compound.

후처리

  1. customUnder a nitrogen atmosphere, in a round-bottom flask equipped with a refluxcondenser
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 6 hours
  4. filtrationThe mixture was filtered through a pad of a diatomaceous earth,and the pad
  5. washwas rinsed with water and CHCl3
  6. extractionwas extracted with three portions of CHCl3
  7. customThe combined organic fractions were dried
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1305e3ea46af43c194c34470a2699d08
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05744480

반응 노트

불러오는 중…