反应详情

78 ml of a 4N solution of hydrochloric acid in dioxane were added to 8.30 g (15.7 mmol) of the carbamate from Example 68A having a purity of 91%, and the mixture was stirred at room temperature for 1 h. The reaction solution was concentrated under reduced pressure and the residue was taken up in 1 N hydrochloric acid. After washing with diethyl ether, the organic phase was concentrated under reduced pressure and the residue was taken up in dichloromethane and extracted repeatedly with 1N hydrochloric acid. The combined aqueous phases were concentrated under reduced pressure, and the residue was dried under high vacuum. Yield: 4.93 g (71% of theory)

1. concentrationThe reaction solution was concentrated under reduced pressure
2. washAfter washing with diethyl ether
3. concentrationthe organic phase was concentrated under reduced pressure
4. extractionextracted repeatedly with 1N hydrochloric acid
5. concentrationThe combined aqueous phases were concentrated under reduced pressure
6. customthe residue was dried under high vacuum