Reacción #1785950

Ecuación de reacción

(±)-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

Disolventes

ethanol

hydrochloric acid dioxane

Condiciones de reacción

Tratamiento posterior

1. 1
   ConcentraciónThe 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
   ExtracciónThe resultant mixture was extracted with methylene chloride
4. 4
   LavadoThe organic layer was washed with brine
5. 5
   Secadodried over anhydrous sodium sulfate
6. 6
   OtroThe solvent was evaporated under reduced pressure, and diisopropyl ether
7. 7
   workup.ADDITIONwas added to the residue for crystallization
8. 8
   OtroCrystals so precipitated
9. 9
   Filtraciónwere collected by filtration, whereby the title compound (1.1 g)
10. 10
    Otrowas obtained

Procedimiento

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.

Fuente