反应详情

温度

-10 °C

A solution of triethylamine (2.7 ml, 0.019 mol) and ethyl chloroformate (2 ml, 0.021 mol) in acetone (40 ml) is added to a solution of the acid obtained in step (i) (3 g, 0.014 mol) in acetone (50 ml) cooled to -10° C. After 1,5 hours at -10° C., concentrated NH4OH (4.5 ml, 0.036 mol) is added dropwise and the reaction mixture is allowed to stand at -10° C. for 1 hour and at room temperature overnight. The solution is concentrated under vacuum, ethyl acetate (150 ml) is added to the obtained residue and the solution is washed sequentially with water, a saturated sodium bicarbonate solution, 6N hydrochloric acid, and water, then it is dried and concentrated to dryness. The residue is triturated with isopropyl ether and filtered thus affording 1.7 g of the above indicated amide; m.p. 136°-138° C.; [α]=+40.2° (c= 1.4%, CHCl3).

1. waitAfter 1,5 hours at -10° C.
2. concentrationThe solution is concentrated under vacuum, ethyl acetate (150 ml)
3. additionis added to the obtained residue
4. washthe solution is washed sequentially with water
5. dry with materiala saturated sodium bicarbonate solution, 6N hydrochloric acid, and water, then it is dried
6. concentrationconcentrated to dryness
7. customThe residue is triturated with isopropyl ether
8. filtrationfiltered thus