HRID2165276

反应详情

EQUATION

反应方程式

HRID 2165276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium carbonate (200g) was dissolved in 300ml of water, 1.5 liters of 1,2-dichloroethane was added, and the mixture was refluxed. A suspension of 178 g of N2 -(t-Butyloxycarbonyl)-O-(methylsulfonyl)-N-(phenylmethoxy)-L-threonineamide in 1.2-dichloroethane was added and the mixture was refluxed for 2 hours. The layers were cooled and the organic layer was evaporated, redissolved in ethyl acetate, washed twice with water, dried (MgSO4) and evaporated again. The oily residue crystallized on treatment with petroleum ether, yielding 76.7 g of the title compound, melting point 78° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. additionwas added
  3. temperaturethe mixture was refluxed for 2 hours
  4. temperatureThe layers were cooled
  5. customthe organic layer was evaporated
  6. dissolutionredissolved in ethyl acetate
  7. washwashed twice with water
  8. dry with materialdried (MgSO4)
  9. customevaporated again
  10. customThe oily residue crystallized on treatment with petroleum ether