HRID280375

反应详情

EQUATION

反应方程式

HRID 280375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (3-oxo-5H-thiazolo[2,3-b]quinazolin-2(3H)-ylidene)acetic acid (1.3 g, 5 mmols), triethylamine (1.5 ml, 0.01 mol), and N-(tert-butyl)benzylamine (0.93 ml, 5 mmols) in 10 ml dichloromethane, was cooled to 10° C. Then, 1.27 g (5 mmols) of N,N-bis(2-oxo-3-oxazolidinyl)phosphorodiamidic chloride was added, and the reaction mixture was stirred at room temperature for 20 hours. Following acidification with dilute hydrochloric acid, the reaction mixture was filtered and the organic layer was washed with water, dried over anhydrous magnesium sulfate, and evaporated to dryness under reduced pressure leaving an orange-yellow solid which was recrystallized from anhydrous ethanol. Yield--0.71 g. Mp 195°-197° C.

WORKUP

后处理

  1. filtrationthe reaction mixture was filtered
  2. washthe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customevaporated to dryness under reduced pressure
  5. customleaving an orange-yellow solid which
  6. customwas recrystallized from anhydrous ethanol
  7. customYield--0.71 g