HRID70106

反应详情

EQUATION

反应方程式

HRID 70106 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under nitrogen a mixture of 74 ml abs. THF and 6 ml abs. methanol is cooled to −70° C. and 2 g sodium hydride (55-65% dispersion) are added. The suspension is stirred for 0.4 hour at ambient temperature. Under nitrogen, 2.05 g N-Boc-L-serine are suspended in 100 ml abs. THF and 40 ml of the prepared sodium ethoxide solution are added. The suspension is stirred for 1 hour at ambient temperature and 1 ml methyliodide are added. After 1 hour the remainder of the sodium ethoxide solution and another 2 ml of methyliodide are added. After 18 hours the reaction mixture is evaporated to dryness. The residue is washed with water and ether and extracted. The water phase is acidified and extracted with ethyl acetate and dichloromethane. 0.52 g of the product are obtained.

WORKUP

后处理

  1. additionUnder nitrogen a mixture of 74 ml abs
  2. stirringThe suspension is stirred for 1 hour at ambient temperature
  3. customAfter 18 hours the reaction mixture is evaporated to dryness
  4. washThe residue is washed with water and ether
  5. extractionextracted
  6. extractionextracted with ethyl acetate and dichloromethane