HRID581375

反应详情

EQUATION

反应方程式

HRID 581375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

15.4 g of p-nitrobenzenesulphonyl chloride are added in portions at 20-25° C. to a stirred suspension of 12.0 g of the alcohol from Example 8 in 35 ml of THF and 7.66 ml of N-methylmorpholine and stirred for 4.5 hours. The suspension is again treated with 0.77 ml of N-methylmorpholine and stirred at 22° C. for 4.5 hours. The mixture is treated with 70 ml of a 2% sodium bicarbonate solution, stirred for 1.5 hours, filtered, the residue is washed with water and ethanol and dried to give 21.4 g (94%) of 98.5% p-nitrobenzenesulphonic acid (4S,5S)-4-benzyl-2-oxo-oxazolidin-5-ylmethyl ester, m.p. 148-149.5° C., [α]D20 : +10.0° (1% acetone).

WORKUP

后处理

  1. stirringstirred at 22° C. for 4.5 hours
  2. stirringstirred for 1.5 hours
  3. filtrationfiltered
  4. washthe residue is washed with water and ethanol
  5. customdried