HRID1856499

反应详情

EQUATION

反应方程式

HRID 1856499 的结构方程式

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To 0.6 Mol of acetic anhydride were added at 25° C. 0.16 Mol 90% HNO3 over 30 minutes. The mixture was stirred for an additional 15 minutes before 0.1 Mol of 1,3-cyclo-heptadiene was added over a 45 minute period, maintaining the temperature at 25° C. The reaction mixture was stirred for an additional 45 minutes before it was poured onto ice water and extracted with methylene chloride. An oily residue (100.5% weight yield) was obtained, which was purified by column chromatography, using silica gel and benzene/ethylacetate 4:1 as eluent. The product has the appearance of a yellow oil.

WORKUP

后处理

  1. additionwas added over a 45 minute period
  2. additionwas poured onto ice water
  3. extractionextracted with methylene chloride
  4. customAn oily residue (100.5% weight yield)
  5. customwas obtained
  6. customwhich was purified by column chromatography