反应详情

温度

30 °C

5′-O-Acetyl-2′,3′-dideoxy-2′,3′-didehydroinosine (100 gm) is added to 25% monomethyl amine (360 ml) at 25-35° C. and stirred for 4-5 hours at 25-35° C. The mass is filtered on a celite bed, washed with methanol (50 ml) and the solvent is distilled off completely under reduced pressure at below 70° C. Methanol (25 ml) is added to the filtrate, the solvent is distilled off completely, and methanol (25 ml) is again added and co-distilled. To the mass, acetone (25 ml) is added, co-distilled, again co-distilled with 25 ml of acetone at below 70° C. and acetone (400 ml) is added. The contents are cooled to 25-35° C., stirred for 2 hours to 2 hours 30 minutes at 25-35° C. Then the reaction mass is cooled to 0-10° C. and stirred for 1 hour to 1 hour 30 minutes. material is filtered, washed with acetone (80 ml) and dried at 55-65° C. to give 62.5 gm of 2′,3′-dideoxy-2′,3′-didehydroinosine (HPLC Purity: 98.14%).

1. filtrationThe mass is filtered on a celite bed
2. washwashed with methanol (50 ml)
3. distillationthe solvent is distilled off completely under reduced pressure at below 70° C
4. additionMethanol (25 ml) is added to the filtrate
5. distillationthe solvent is distilled off completely
6. additionmethanol (25 ml) is again added
7. additionTo the mass, acetone (25 ml) is added
8. customagain co-distilled with 25 ml of acetone at below 70° C.
9. additionacetone (400 ml) is added
10. temperatureThe contents are cooled to 25-35° C.
11. stirringstirred for 2 hours to 2 hours 30 minutes at 25-35° C
12. temperatureThen the reaction mass is cooled to 0-10° C.
13. stirringstirred for 1 hour to 1 hour 30 minutes
14. filtrationmaterial is filtered
15. washwashed with acetone (80 ml)
16. customdried at 55-65° C.