HRID874798

反应详情

EQUATION

反应方程式

HRID 874798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trimellitic acid anhydride chloride (50 g, 0.240 mol) is dissolved in 150 mL acetone in a 3-neck flask under nitrogen. The flask is cooled in an ice bath. A solution of AFM-caprolactone intermediate (82.05 g, 0.12 mol), and pyridine (19.0 g, 0.240 mol) in 80 ml of acetone is added slowly through a dropping funnel while continuously stirring the cold solution. After addition is completed, the flask contents are continuously stirred at room temperature for 4 hours. Water (4.32 g, 0.240 mol) is added and the solution is stirred continuously at room temperature overnight. The solids formed are removed by vacuum filtration and washed with acetone. The filtrate is concentrated and dried to yield the product

WORKUP

后处理

  1. temperatureThe flask is cooled in an ice bath
  2. additionAfter addition
  3. stirringthe flask contents are continuously stirred at room temperature for 4 hours
  4. stirringthe solution is stirred continuously at room temperature overnight
  5. customThe solids formed
  6. customare removed by vacuum filtration
  7. washwashed with acetone
  8. concentrationThe filtrate is concentrated
  9. customdried
  10. customto yield the product