反应详情

In a manner similar to Example 1B, 1.0 g. of 91% sodium hydride was added over a period of one hour to a solution of 3.0 g. (0.015 mole) of N-methylsaccharin and 2.6 g. (0.017 mole) of 2-methoxyethyl chloroacetate in 15 ml. of dimethylformamide at 35° C. The exothermic reaction (55° C.) was allowed to stir for 2 hours after the addition was complete, and was then quenched in 5% hydrochloric acid solution and the product extracted with methylene chloride. The residue, remaining after the solvent was removed, was dissolved in 10 ml. of warm dimethylformamide and added to 100 ml. of 2% hydrochloric acid. The cooled suspension was stirred for 30 minutes and filtered. Drying of the filtered material gave 1.12 g. (24%) of the product identical with that prepared in Example 1B.

1. customat 35° C
2. customThe exothermic reaction (55° C.)
3. additionafter the addition
4. customwas then quenched in 5% hydrochloric acid solution
5. extractionthe product extracted with methylene chloride
6. customwas removed
7. dissolutionwas dissolved in 10 ml
8. additionof warm dimethylformamide and added to 100 ml
9. stirringThe cooled suspension was stirred for 30 minutes
10. filtrationfiltered
11. customDrying of the filtered material
12. customgave 1.12 g