反応 #1785950

反応方程式

(±)-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

溶媒

ethanol

hydrochloric acid dioxane

反応条件

後処理

1. 1
   濃縮The 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
   抽出The resultant mixture was extracted with methylene chloride
4. 4
   洗浄The organic layer was washed with brine
5. 5
   乾燥dried over anhydrous sodium sulfate
6. 6
   その他The solvent was evaporated under reduced pressure, and diisopropyl ether
7. 7
   workup.ADDITIONwas added to the residue for crystallization
8. 8
   その他Crystals so precipitated
9. 9
   ろ過were collected by filtration, whereby the title compound (1.1 g)
10. 10
    その他was obtained

実験手順

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.

出典