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

HRID 277890

반응식

HRID 277890 반응식
[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]

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 27975912-Methyl-2-phenylpropanenitrileHCID 21226445Aluminium lithium hydride

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5f9a22167e3c4f08bf9905d0420e8268
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06358974B1

연결된 노트

불러오는 중…