HRID421189

反应详情

EQUATION

反应方程式

HRID 421189 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared according to the method described by H. H. Otto, Helvetica Chimica Acta, 2004, 87, 90. To an ice cooled solution of N-(phenylmethyl)-D-serine (8.90 g, 45.59 mmol) in 2N NaOH solution (50 mL) was added chloroacetyl chloride (4.36 mL, 54.71 mmol), dropwise over 15 minutes. The reaction was stirred for 30 minutes before adding 30% NaOH solution (4.5 g in 15 mL) and stirring at R.T. for 2 and ½ hours. It was cooled in an ice bath before adding c.HCl solution to pH<1. solid precipitated out. Filtered. Suspended in isopropanol and heated at reflux for 10 minutes. Filtered hot. Solvent evaporated to afford a pale yellow solid. Triturated with Et2O to afford the title compound as a cream solid in 29% yield.

WORKUP

后处理

  1. customThe title compound was prepared
  2. stirringstirring at R.T. for 2 and ½ hours
  3. temperatureIt was cooled in an ice bath
  4. additionbefore adding c
  5. customsolid precipitated out
  6. filtrationFiltered
  7. temperatureheated
  8. temperatureat reflux for 10 minutes
  9. filtrationFiltered hot
  10. customSolvent evaporated
  11. customto afford a pale yellow solid
  12. customTriturated with Et2O