反应详情

温度

5 °C

0.9 g of sodium hydroxide is added to a solution of 3 g of N-methylleucine in 70 ml of water and 40 ml of tetrahydrofuran. The medium is then cooled to 5° C. and a solution of 7.3 g of 2-(5-chloro-2,3-dihydro-2-oxo-3-phenyl-3-benzofuranyl)acetyl chloride in 50 ml of tetrahydrofuran and a solution of 0.9 g of sodium hydroxide in 22.7 ml of water are then added simultaneously in small portions so as to maintain the pH at 12. The mixture is stirred for 3 hours at room temperature and 22.7 ml of N hydrochloric acid are added. The medium is concentrated and the precipitate obtained is filtered off and dissolved hot in an ethanol/methanol (50:50) mixture. The solution is filtered and the filtrate evaporated. A crystalline product is obtained.

1. temperatureto maintain the pH at 12
2. concentrationThe medium is concentrated
3. customthe precipitate obtained
4. filtrationis filtered off
5. dissolutiondissolved hot in an ethanol/methanol (50:50) mixture
6. filtrationThe solution is filtered
7. customthe filtrate evaporated
8. customA crystalline product is obtained