Potassium Sodium Tartrate → 1-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine

HRID 35710

반응식

HRID 35710 반응식
[C:1](=[N:15]O)([C:3]1([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[C:9]([Cl:14])[CH:8]=2)[CH2:6][CH2:5][CH2:4]1)[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+].[OH-].[Na+]>CCOCC.O>[Cl:14][C:9]1[CH:8]=[C:7]([C:3]2([CH:1]([NH2:15])[CH3:2])[CH2:6][CH2:5][CH2:4]2)[CH:12]=[CH:11][C:10]=1[Cl:13]

참가 물질

7

반응물 4

HCID 9357Potassium Sodium TartrateHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 860311131-Acetyl-1-(3,4-dichlorophenyl)cyclobutane oxime

생성물 1

HCID 130831401-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매2회

실험 절차

A solution of the oxime prepared above (4.0 g) in ether (50 ml) was added slowly to a stirred suspension of lithium aluminium hydride (0.9 g) in ether (50 ml) under nitrogen. The mixture was heated under reflux for one hour and, after cooling, water and then a 20% aqueous solution of Rochelle's salt (potassium sodium tartrate tetrahydrate) (27 ml) and a 10% aqueous solution of sodium hydroxide (6 ml) added. The reaction mixture was stirred for one hour and then continuously extracted with ether during eighteen hours. The ether extract was dried and the ether removed to leave a solid from which 1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine was separated by high pressure liquid chromatography. The product was identified by standard analytical techniques as the compound of Example 1 in the form of its free base.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for one hour
  3. temperatureafter cooling
  4. extractioncontinuously extracted with ether during eighteen hours
  5. extractionThe ether extract
  6. customwas dried
  7. customthe ether removed

출처 및 근거

ORD 기록
ord-f58e48150f6d4f5bacb8a34d603b8129
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767790

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