反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
19.1 g of sodium 1,1,1,3,3,3-hexamethyldisilazanate are added to a solution, cooled to -50° C., of 10 g of (4S,5S)-4-methyl-5-phenyl-3-[(2-methoxyphenyl)acetyl]oxazolidin-2-one in 150 cm3 of tetrahydrofuran, the mixture is stirred at this temperature for 45 minutes and 7.72 cm3 of methyl iodide are then added. The reaction mixture is then stirred at room temperature for 15 hours, subsequently diluted with ethyl acetate, washed with 50 cm2 of water and then with 50 cm3 of an aqueous saturated solution of sodium chloride, dried over magnesium sulphate and concentrated to dryness under reduced pressure (2.7 kPa). The residue obtained is crystallized in isopropyl ether, filtered off and dried. 4.2 g of (4S,5S)-4-methyl-5-phenyl-3-[(S)-2-(2-methoxyphenyl)propionyl]oxazolidin-2-one are obtained in the form of a white solid.
WORKUP
后处理
- stirringThe reaction mixture is then stirred at room temperature for 15 hours
- washwashed with 50 cm2 of water
- dry with materialwith 50 cm3 of an aqueous saturated solution of sodium chloride, dried over magnesium sulphate
- concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
- customThe residue obtained
- customis crystallized in isopropyl ether
- filtrationfiltered off
- customdried