反应详情

A solution of 4-chloro-5-iodo-7H-pyrrolo[2,3-d]pyrimidine (20.0 g) in DMF (50 ml) was slowly added to a solution of sodium hydride (3.4 g) in DMF (190 ml) under ice cooling. Thereafter, 2-(trimethylsilyl)ethoxymethyl chloride (13.3 ml) was added thereto, and stirred at the same temperature for 2 hours. 2-(Trimethylsilyl)ethoxymethyl chloride (1.3 ml) was additionally added to the reaction mixture, and stirred at room temperature for 1 hour. The reaction mixture was poured into water (600 ml), and stirred at room temperature for 15 minutes. The resulting precipitate was collected by filtration and washed with water and diisopropyl ether, followed by dissolution with ethyl acetate again. Insoluble matter was then filtered off by filtration. The solvent of the filtrate was distilled off under reduced pressure. Heptane was added to the resulting residue to collect the precipitate by filtration. The precipitate was washed with heptane, and dried under reduced pressure to obtain the title compound (21.2 g) as a white solid.

1. stirringstirred at room temperature for 1 hour
2. stirringstirred at room temperature for 15 minutes
3. filtrationThe resulting precipitate was collected by filtration
4. washwashed with water and diisopropyl ether
5. dissolutionfollowed by dissolution with ethyl acetate again
6. filtrationInsoluble matter was then filtered off by filtration
7. distillationThe solvent of the filtrate was distilled off under reduced pressure
8. additionHeptane was added to the resulting residue
9. customto collect the precipitate
10. filtrationby filtration
11. washThe precipitate was washed with heptane
12. customdried under reduced pressure