HRID434472

反应详情

EQUATION

反应方程式

HRID 434472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

4-t-Butyl-2,6-dinitrochlorobenzene (1.8 grams; 0.007 mole), N-(1,3-dioxolan-2-yl)methyl ethylamine (1.83 grams; 0.014 mole) and toluene (50 ml) were placed in a glass reaction vessel equipped with a stirrer, heating mantle, reflux condenser and thermometer. The reaction mixture was heated to 90° C. and maintained at this temperature with stirring for 72 hours. Diethyl ether (50 ml) was added to the cooled reaction mixture, which was filtered and evaporated to a volume of 10 cc. The residue was chromatographed on silica to remove unreacted starting material. The product (1.7 grams) was obtained as an oil which solidified on standing (73°-74° C. melting point). The product was analyzed for C16H23N3O6 :

WORKUP

后处理

  1. customequipped with a stirrer
  2. temperatureheating mantle
  3. temperaturereflux condenser
  4. temperaturemaintained at this temperature
  5. filtrationwas filtered
  6. customevaporated to a volume of 10 cc
  7. customThe residue was chromatographed on silica
  8. customto remove unreacted