Methanol → 3,5-Bis(trifluoromethyl)benzylamine

HRID 279488

反応式

HRID 279488 の反応式
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1)[C:6]#[N:7].CO.[H][H]>[Pd]>[F:1][C:2]([F:15])([F:16])[C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([C:11]([F:14])([F:12])[F:13])[CH:10]=1)[CH2:6][NH2:7]

参加物

5

反応物 3

HCID 887MethanolHCID 967463,5-Bis(trifluoromethyl)benzonitrileHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 5210993,5-Bis(trifluoromethyl)benzylamine収率 87%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

At first, a 1-liter autoclave equipped with a mechanical stirrer was charged with 50 g (0.21 mol) of 3,5-bis(trifluoromethyl)benzonitrile, 200 ml of 2M-ammoniacal methanol solution (containing 400 mmol of ammonia), and 3 g of a catalyst (i.e., a carbon powder (50% wet) carrying thereon 5% palladium), followed by introduction of hydrogen to have a pressure of 1 MPa. Then, the reaction mixture was stirred, while the reaction temperature was maintained at 20° C. and while hydrogen was gradually introduced into the autoclave in a manner to maintain the total pressure at 1 MPa. After conducting the reaction for 5.3 hr, the reaction was stopped, followed by removing the catalyst by filtration. As a result of analyzing the obtained reaction liquid by gas chromatography, 3,5-bis(trifluoromethyl)benzylamine was formed at a yield of 87.0%.

後処理

  1. customAt first, a 1-liter autoclave equipped with a mechanical stirrer
  2. additionwas gradually introduced into the autoclave in a manner
  3. temperatureto maintain the total pressure at 1 MPa
  4. customthe reaction for 5.3 hr
  5. customby removing the catalyst
  6. filtrationby filtration
  7. customAs a result
  8. customthe obtained reaction liquid by gas chromatography

出典と根拠

ORDレコード
ord-94b473c162ce4457a2b580d2875c239c
出典データセット
uspto-grants-2002_03
特許番号
US06362372B1

関連ノート

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