HRID1262555

反应详情

EQUATION

反应方程式

HRID 1262555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-Hydroxyacridine (1.90 grams; 0.01 mole), triethylamine (1.01 grams; 0.01 mole), tetrahydrofuran (30 ml) and toluene (20 ml) were charged into a glass reaction vessel equipped with a mechanical stirrer and thermometer. The mixture was cooled to about 0° C. and O-ethyl S-propyl phosphorochloridothioate (2.01 grams; 0.01 mole) dissolved in toluene (23 ml) was added with stirring over a period of about 20 minutes. After the addition was completed stirring was continued for 3 hours allowing the mixture to warm up to room temperature. Stirring was continued overnight. After this time the reaction mixture was filtered to remove triethylamine hydrochloride. The filtrate was washed, treated with charcoal and stripped of solvent leaving yellow/green oil as the residue. This residue was subjected to flash chromatography using ethyl acetate as the eluant to yield the desired product O-ethyl O-acridin-2-yl S-propyl phosphorothioate as a yellow brown oil.

WORKUP

后处理

  1. customequipped with a mechanical stirrer
  2. additionwas added
  3. additionAfter the addition
  4. stirringwas completed stirring
  5. waitwas continued for 3 hours
  6. temperatureto warm up to room temperature
  7. stirringStirring
  8. waitwas continued overnight
  9. filtrationAfter this time the reaction mixture was filtered
  10. customto remove triethylamine hydrochloride
  11. washThe filtrate was washed
  12. additiontreated with charcoal
  13. customleaving yellow/green oil as the residue