HRID280373

反应详情

EQUATION

反应方程式

HRID 280373 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1.30 g (5 mmols) (3-oxo-5H-thiazolo[2,3-b]quinazolin-2(3H)-ylidene)acetic acid, 1.27 g (5 mmols) N,N-bis(2-oxo-3-oxazolidinyl)phosphorodiamidic chloride, 0.49 g (5.2 mmols) phenol, and 1.10 g (10 mmols) triethylamine, in 10 ml dichloromethane was stirred at room temperature, under nitrogen atmosphere for 18 hours. Then, 10 ml of water (made slightly basic with sodium bicarbonate) were added. The precipitate was filtered of and the filtrate was dried over anhydrous magnesium sulfate, and evaporated to dryness under reduced pressure. The residual orange-yellow solid was recrystallized from anhydrous ethanol. Yield--0.62 g. Mp 194°-195° C.

WORKUP

后处理

  1. additionwere added
  2. filtrationThe precipitate was filtered of and the filtrate
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. customevaporated to dryness under reduced pressure
  5. customThe residual orange-yellow solid was recrystallized from anhydrous ethanol
  6. customYield--0.62 g