反应详情

温度

90 °C

0.3 g (10 mmol) of sodium hydride (80%) are stirred in 15 ml of tetrahydrofuran and 1.42 g (10 mmol) of 4-chlorobenzyl alcohol in 10 ml of tetrahydrofuran are added dropwise. The resulting clear solution is evaporated to dryness and a solution of 2.02 g (6.5 mmol) of 3-chloro-3-(3,4-dimethoxyphenyl)-1-morpholin-4-ylprop-2-en-1-one in 25 ml of dimethylformamide is added. The mixture is stirred at 90° C. for 20 hours. The solvent is then evaporated and the residue shaken with toluene/water. The organic phase is separated, washed with water, dried and purified over a flash column with 40 g of silicagel. Elution is carried out with toluene containing 10, 20 and 30% of acetone. The fractions with the TLC Rf-values 0.45 and 0.31 (toluene/acetone 7:3) are collected and evaporated.

1. customThe resulting clear solution is evaporated to dryness
2. customThe solvent is then evaporated
3. stirringthe residue shaken with toluene/water
4. customThe organic phase is separated
5. washwashed with water
6. customdried
7. custompurified over a flash column with 40 g of silicagel
8. washElution
9. customThe fractions with the TLC Rf-values 0.45 and 0.31 (toluene/acetone 7:3) are collected
10. customevaporated