反应详情

温度

5 °C

Twenty grams of [R-(R*,R*)]-5-(3-chlorophenyl)-3-[2-(3,4-dimethyloxyphenyl)-1-methylethyl]-2-oxazolidinone, prepared by the procedure described in U.S. Pat. No. 5.061,727, is dissolved in 100 ml of methylene chloride and cooled to 5° C. under a stream of argon. Ten ml of boron tribromide in 10 ml of methylene chloride is added dropwise over 25 minutes. The reaction mixture is stirred for 20 minutes at 0°-5° C. One hundred and fifty ml of methyl alcohol is added over 40 minutes and the reaction is allowed to warm to room temperature over 1 hour. The solvent is removed by distillation (pot temperature 90° C.) leaving an oil in the bottom of the flask. The reaction flask is charged with 36.9 g of methyl alcohol, cooled to room temperature and 148 g of water is added over 1.5 hours. The reaction is stirred at room temperature for 72 hours, followed by cooling to 5° C. and stirring at this temperature for 1 hour. The resulting precipitate is collected, rinsed with water, and dried to give 17.1 g of the desired product (Yield 92.7% theory).

1. temperatureto warm to room temperature over 1 hour
2. customThe solvent is removed by distillation (pot temperature 90° C.)
3. customleaving an oil in the bottom of the flask
4. temperaturecooled to room temperature
5. stirringThe reaction is stirred at room temperature for 72 hours
6. temperatureby cooling to 5° C.
7. stirringstirring at this temperature for 1 hour
8. customThe resulting precipitate is collected
9. washrinsed with water
10. customdried