Sodium Hydroxide → 2-((Dimethylamino)methyl)-1-(3-methoxyphenyl)cyclohexanol

HRID 1296Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1296
Cl.[CH3:2][N:3]([CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=1)[OH:12])[CH3:4].[OH-].[Na+]>O>[CH3:4][N:3]([CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=1)[OH:12])[CH3:2]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 9971980Cyclohexanol, 2-((dimethylamino)methyl)-1-(3-methoxyphenyl)-, hydrochloride (1:1)

Produkt 1

HCID 55232-((Dimethylamino)methyl)-1-(3-methoxyphenyl)cyclohexanolAusbeute 99,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

3 kg (10 mole) (1RS,2RS)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol hydrochloride (1) were suspended in 4800 ml water and treated with 1.6 kg crushed ice. 1300 ml of 36-38% (technical) caustic soda solution were added drop-wise with stirring. The mixture was subsequently extracted with 7000 ml dichloromethane, and was extracted with a further 2000 ml dichloromethane after phase separation. The combined organic phases were dried over sodium sulphate. After removing the solvent by distillation, 2630 g (99% theoretical) of (1RS,2RS)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol were obtained as a syrup.

Aufarbeitung

  1. additiontreated with 1.6 kg
  2. customcrushed ice
  3. extractionThe mixture was subsequently extracted with 7000 ml dichloromethane
  4. extractionwas extracted with a further 2000 ml dichloromethane
  5. customafter phase separation
  6. dry with materialThe combined organic phases were dried over sodium sulphate
  7. customAfter removing the solvent
  8. distillationby distillation

Quellen und Nachweise

ORD-Eintrag
ord-822a168440d44234b23b8b29fa23f00d
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05723668

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