HRID2255676

反应详情

EQUATION

反应方程式

HRID 2255676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution containing 0.6 g (0.0016 mole) of N-(4,4,4-trinitrobutyryl)-N'-(perfluoropropionyl)hydrazine and 0.8 g (0.0038 mole) of phosphorus pentachloride in 7 mL of 1,2-dichloroethane was held at reflux temperature for 4 hours before the volatiles were removed to give an oil residue. The residue was dissolved in CH2Cl2, washed with water, and chromatographed on Silica gel 40 (CH2Cl2 as eluent) to give the product, 2-(3,3,3-trinitropropyl)-5-(perfluoroethyl)-1,3,4-oxadiazole, 0.4 g (70%), mp 36°-38° C. 1H NMR (acetone-d6): 3.80 (m, 2H), 4.20 (m, 2H).

WORKUP

后处理

  1. temperatureat reflux temperature for 4 hours before the volatiles
  2. customwere removed
  3. customto give an oil residue
  4. washwashed with water
  5. customchromatographed on Silica gel 40 (CH2Cl2 as eluent)