反应详情

温度

-10 °C

Add 3.1 g (0.0773 mol) of sodium hydride in portions to a solution at 0° C. of 11.9 ml (0.0736 mol) of diethyl cyanomethylphosphonate in 400 ml of THF. Cool the mixture to −10° C. and add dropwise a suspension of 21.3 g (0.0736 mol) of 2-formyl-4,5-dimethoxyphenyl dimethylsulphamate in 200 ml of THF. Stir for 30 minutes and hydrolyse with 600 ml of a solution of sodium hydrogen carbonate and water (50/50) and then extract the solution twice with 300 ml of toluene each time. The organic phase is washed with 100 ml of water and 100 ml of saturated aqueous NaCl solution and then dried over MgSO4, filtered and evaporated to dryness. The residue obtained is crystallised in 80 ml of diisopropyl ether at ambient temperature and then filtered and washed with 20 ml of diisopropyl ether and dried in vacuo. 18.4 g of title product are obtained.

1. additionadd dropwise
2. extractionextract the solution twice with 300 ml of toluene each time
3. washThe organic phase is washed with 100 ml of water and 100 ml of saturated aqueous NaCl solution
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated to dryness
7. customThe residue obtained
8. customis crystallised in 80 ml of diisopropyl ether at ambient temperature
9. filtrationfiltered
10. washwashed with 20 ml of diisopropyl ether
11. customdried in vacuo