反应详情

To a mixture of methyl 5-{4-[(4-hydroxymethyl-2-methoxyphenoxy)methyl]-5-methyl-1,3-oxazol-2-yl}-2-methylbenzoate (1.16 g) and toluene (50 mL) was added thionyl chloride (0.38 g), and the mixture was heated under reflux for 1 hr. The reaction mixture was concentrated and ethyl acetate was added to the residue. The organic layer was washed successively with saturated aqueous sodium hydrogen carbonate and saturated brine, dried over anhydrous magnesium sulfate and concentrated to give methyl 5-{4-[(4-chloromethyl-2-methoxyphenoxy)methyl]-5-methyl-1,3-oxazol-2-yl}-2-methylbenzoate (1.18 g, yield 98%) as colorless crystals. Recrystallization from ethyl acetate-hexane gave colorless prism crystals. melting point: 139-140° C.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 1 hr
3. concentrationThe reaction mixture was concentrated
4. additionethyl acetate was added to the residue
5. washThe organic layer was washed successively with saturated aqueous sodium hydrogen carbonate and saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated