反应详情

温度

5 °C

1,3-Dioxolan-2 ylmethylamine (4 grams; 0.04 mol), triethylamine (5 ml) and dichloromethane (150 ml) were placed in a 3-necked glass reaction flask equipped with stirrer, thermometer and reflux condenser and cooled to 5° C. 2[4-(5-Trifluoromethyl-2-pyridinyloxy)-phenoxy]propanoic acid chloride (9 grams; 0.027 mol) in dichloromethane (30 ml) was added in a five minute time period. The reaction mixture was stirred for 1 hour at 5° C.-20° C., washed with water, passed through phase separating paper and concentrated to a dark gum (10.5 grams). The product was chromatographed through Florisil clay (100 ml), using hexane-ethyl acetate solvent mixtures. The desired product was isolated as a yellow gum (3.0 grams) and had the following elemental analysis:

1. customequipped with stirrer
2. temperaturethermometer and reflux condenser
3. washwashed with water
4. customseparating paper
5. concentrationconcentrated to a dark gum (10.5 grams)
6. customThe product was chromatographed through Florisil clay (100 ml)