Reaktion #1785950

Reaktionsgleichung

(±)-1-tert-butylcarbonylmethyl-2-oxo-3-tert-butoxycarbonylamino-5-cyclohexyl-1,3,4,5-tetrahy dro-2H-1,5-benzodiazepine

→

(±)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine

Lösungsmittel

ethanol

hydrochloric acid dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONa saturated aqueous solution of sodium hydrogencarbonate was added to the residue for neutralization
3. 3
   ExtraktionThe resultant mixture was extracted with methylene chloride
4. 4
   WaschenThe organic layer was washed with brine
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   SonstigeThe solvent was evaporated under reduced pressure, and diisopropyl ether
7. 7
   workup.ADDITIONwas added to the residue for crystallization
8. 8
   SonstigeCrystals so precipitated
9. 9
   Filtrationwere collected by filtration, whereby the title compound (1.1 g)
10. 10
    Sonstigewas obtained

Vorschrift

To a solution of (±)-1-tert-butylcarbonylmethyl-2-oxo-3-tert-butoxycarbonylamino-5-cyclohexyl-1,3,4,5-tetrahy dro-2H-1,5-benzodiazepine (2.2 g) in ethanol (10 mL), 4 N hydrochloric acid-dioxane solution (10 mL) was added. The resulting mixture was stirred at 50° C. for 30 minutes. The reaction mixture was concentrated under reduced pressure, and a saturated aqueous solution of sodium hydrogencarbonate was added to the residue for neutralization. The resultant mixture was extracted with methylene chloride. The organic layer was washed with brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and diisopropyl ether was added to the residue for crystallization. Crystals so precipitated were collected by filtration, whereby the title compound (1.1 g) was obtained.

Quelle