Water → 2-Methyl-2-phenylpropan-1-amine

HRID 277890

反応式

HRID 277890 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([CH3:11])[C:9]#[N:10].O.[OH-].[Na+]>C(OCC)C>[CH3:11][C:8]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([CH3:7])[CH2:9][NH2:10]

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 27975912-Methyl-2-phenylpropanenitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 2106022-Methyl-2-phenylpropan-1-amine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To a stirred suspension of lithium aluminium hydride (4.85 g, 0.128 mol) in anhydrous diethyl ether (245 ml) at ambient temperature under argon was added a solution of α,α-dimethylphenylacetonitrile (12.4 g, 0.085 mol) in anhydrous diethyl ether (105 ml) dropwise over 0.5 hour. The resultant was heated at reflux for 3 hours, cooled to ambient temperature and treated with water (4.6 ml), 15% aqueous sodium hydroxide (4.6 ml) and water (13.8 ml) dropwise sequentially. The mixture was stirred for 1.5 hours, filtered and the filtrate dried (Na2SO4) and treated with 1N hydrogen chloride in ether (100 ml). The precipitated solid was filtered and dried to afford the title compound as the hydrochloride salt (9.4 g, 52%).

後処理

  1. temperatureThe resultant was heated
  2. temperatureat reflux for 3 hours
  3. filtrationfiltered
  4. dry with materialthe filtrate dried (Na2SO4)
  5. additiontreated with 1N hydrogen chloride in ether (100 ml)
  6. filtrationThe precipitated solid was filtered
  7. customdried

出典と根拠

ORDレコード
ord-5f9a22167e3c4f08bf9905d0420e8268
出典データセット
uspto-grants-2002_03
特許番号
US06358974B1

関連ノート

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