反应详情

8.5 g (0.1 mole) of cyanoacetic acid, 10.43 g (0.1 mole) of trimethylsilylmethanol, 30.66 g (0.12 mole) of 2-chloro-1-methylpyridinium iodide, 24.3 g (0.24 mole) of triethylamine and 200 ml of tetrahydrofuran were placed in a reaction vessel and reaction was allowed to take place at 50° C. for 3 hours in an argon atmosphere. Thereafter, a 10% aqueous sodium thiosulfate solution was added, followed by extraction with ether. An organic layer obtained was washed with a 10% aqueous sodium thiosulfate solution and then with water, then dried overnight with anhydrous magnesium. Thereafter, the desiccant was filtered off and the solvent was removed under a reduced pressure, followed by vacuum distillation to afford 14.6 g of trimethylsilylmethyl α-cyanoacetate (NCCH2CO2CH2SiMe3) (b.p. 81°-82° C./2 mmHg, yield 85%).

1. customreaction
2. customat 50° C.
3. customfor 3 hours
4. extractionfollowed by extraction with ether
5. customAn organic layer obtained
6. washwas washed with a 10% aqueous sodium thiosulfate solution
7. dry with materialwith water, then dried overnight with anhydrous magnesium
8. filtrationThereafter, the desiccant was filtered off
9. customthe solvent was removed under a reduced pressure
10. distillationfollowed by vacuum distillation