反应详情

1.54 g (10 mmols) of the product obtained by the procedure described in (1b) are reacted with 1.8 mL of acryloyl chloride, in the presence of 4.2 mL of triethylamine in 100 mL of tetrahydrofuran. The addition is performed dropwise and under cooling in an ice bath. After the addition is complete, the reaction mixture is stirred at room temperature for several hours. The solvent is evaporated under vacuum and then 100 mL of water are added to the solid residue to dissolve the TEA.HCl salt. The mixture is then extracted with 3×100 mL CHCl3, the organic phases are combined, dried over MgSO4 and the solvent is finally evaporated in vacuo. A white solid is finally obtained and there is no need for further purification.

1. additionThe addition
2. temperatureunder cooling in an ice bath
3. additionAfter the addition
4. customThe solvent is evaporated under vacuum
5. addition100 mL of water are added to the solid residue
6. dissolutionto dissolve the TEA
7. extractionThe mixture is then extracted with 3×100 mL CHCl3
8. dry with materialdried over MgSO4
9. customthe solvent is finally evaporated in vacuo
10. customA white solid is finally obtained
11. customfor further purification