HRID1017121

反应详情

EQUATION

反应方程式

HRID 1017121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of maleic anhydride (0.05 mole) in acetic acid (20 mL) was mixed with a solution of ε-Amino-n-caproic acid (0.05 mole) in acetic acid (50 mL) and stirred at room temperature for 2 hours. An additional amount of acetic acid (150 mL) was added and the reaction mixture refluxed for 16 hours. The reaction mixture was evaporated under vacuo to an oil and chloroform was then added (50 mL). The solution was left to stand for 16 hours at room temperature whereupon impurities were precipitated out of the solution. The precipitate was filtered and the filtrate was collected, evaporated under vacuo and chromatographed on silica gel using chloroform:acetic acid (95:5) to give 6-Maleimidocaproic acid 23 (8 g).

WORKUP

后处理

  1. temperaturethe reaction mixture refluxed for 16 hours
  2. customThe reaction mixture was evaporated under vacuo to an oil and chloroform
  3. additionwas then added (50 mL)
  4. waitThe solution was left
  5. waitto stand for 16 hours at room temperature whereupon impurities
  6. customwere precipitated out of the solution
  7. filtrationThe precipitate was filtered
  8. customthe filtrate was collected
  9. customevaporated under vacuo
  10. customchromatographed on silica gel