HRID1599131

反应详情

EQUATION

反应方程式

HRID 1599131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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 then 7.72 cm3 of methyl iodide are added. The reaction mixture is subsequently stirred at room temperature for 15 hours, then diluted with ethyl acetate, washed with 50 cm3 of water followed by 50 cm3 of saturated aqueous sodium chloride solution, dried over magnesium sulphate and concentrated to dryness under reduced pressure (2.7 kPa). The residue obtained is recrystallized from isopropyl ether, drained 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

  1. stirringThe reaction mixture is subsequently stirred at room temperature for 15 hours
  2. washwashed with 50 cm3 of water
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
  5. customThe residue obtained
  6. customis recrystallized from isopropyl ether
  7. customdried