Hydrochloric Acid → 2-Phenylpropylamine hydrochloride

HRID 420823

反応式

HRID 420823 の反応式
C(O)C.[C:4]1([CH:10]([CH3:13])[C:11]#[N:12])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[ClH:14].[H][H]>C(OC)(C)(C)C>[ClH:14].[C:4]1([CH:10]([CH3:13])[CH2:11][NH2:12])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 157612-PhenylpropionitrileHCID 178418361HCID 178418361、化合物

生成物 1

HCID 893322-Phenylpropylamine hydrochloride収率 76.2%

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒

実験手順

Charge to an autoclave hydrogenation apparatus under nitrogen water-wet 5% palladium on carbon (453 g), ethanol (6.36 L), 2-phenylpropionitrile (636 g, 4.85 moles) and finally concentrated (12M) hydrochloric acid (613 g, 5.6 mole). Stir the mixture rapidly and pressurize to 75 to 78 psi with hydrogen. Heat the mixture 50° C. to 64° C. for 3 hours. Depressurize and filter the reaction mixture to afford two lots of filtrate. Concentrate filtrates under reduced pressure to approximately 400 mL each. Add methyl tert-butyl ether (MTBE) (2.2 L each) to each lot. Stir the precipitate overnight. Filter and wash solids with fresh MTBE (100 mL) and dry overnight. Combine the lots to afford 2-phenyl-1-propylamine HCl (634.4 g, 76.2%) as a white powder.

後処理

  1. additionCharge to an autoclave hydrogenation apparatus under nitrogen water-wet 5% palladium on carbon (453 g)
  2. temperatureHeat the mixture 50° C. to 64° C. for 3 hours
  3. filtrationDepressurize and filter the reaction mixture
  4. customto afford two lots of filtrate
  5. stirringStir the precipitate overnight
  6. filtrationFilter
  7. washwash solids with fresh MTBE (100 mL)
  8. customdry overnight

出典と根拠

ORDレコード
ord-dc753b3f3cf94d54bf0285b696229e54
出典データセット
uspto-grants-2012_01
特許番号
US08097652B2

関連ノート

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