反应详情

Hydrogen chloride gas was introduced into a solution containing 15.0 g of N2 -tert-butoxycarbonyl-N1 -[2-(4-cyanophenoxy)-1-methylethyl]-L-isoleucinamide dissolved in 300 mL of methylene chloride for 1 hour at room temperature. After completion of the reaction, the methylene chloride was removed under reduced pressure, thus obtaining a crude crystal. 200 ml of a saturated aqueous solution of sodium bicarbonate and 200 ml of methylene chloride were added to the crude crystal, and the mixture was stirred for 30 minutes and extracted with methylene chloride. The organic layer was washed with water, and dried over anhydrous sodium sulfate. The methylene chloride was removed under reduced pressure. The obtained crude product was washed with acetone to afford 10.0 g of the desired product (yield: 90%). Melting point: 64°-67° C.

1. customAfter completion of the reaction
2. customthe methylene chloride was removed under reduced pressure
3. customthus obtaining a crude crystal
4. extractionextracted with methylene chloride
5. washThe organic layer was washed with water
6. dry with materialdried over anhydrous sodium sulfate
7. customThe methylene chloride was removed under reduced pressure
8. customThe obtained crude product
9. washwas washed with acetone