反应详情

In 100 ml of methylene chloride were dissolved 6.15 g of 2-[3-(2-nitrophenoxy)phenoxy]propionic acid and 4.2 g of triethylamine, followed by dropwise addition of 2.5 g of ethyl chloroformate at a temperature not exceeding 0° C., and the mixture was further stirred at the same temperature for 30 minutes. The reaction mixture was poured into previously ice-cooled methylene chloride (120 ml) saturated with ammonia gas and the mixture was then stirred at room temperature for 30 minutes. The methylene chloride layer was washed with water (twice), dried and concentrated and the residue was crystallized from methanol and isopropyl ether to give 3.3 g of the title compound.

1. customexceeding 0° C.
2. additionThe reaction mixture was poured into previously ice-
3. stirringthe mixture was then stirred at room temperature for 30 minutes
4. washThe methylene chloride layer was washed with water (twice),
5. customdried
6. concentrationconcentrated
7. customthe residue was crystallized from methanol and isopropyl ether