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

HRID 1600200

反応式

HRID 1600200 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1305e3ea46af43c194c34470a2699d08
出典データセット
uspto-grants-1998_04
特許番号
US05744480

関連ノート

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