HRID1051845

反应详情

EQUATION

反应方程式

HRID 1051845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of (5-hydroxy-1,3-phenylene)dimethanol (7.27 g, 47 mmol, 1 eq.) in 200 mL of acetonitrile at room temperature, 2-(4-bromobutyl)isoindoline-1,3-dione (1.2 eq.) and potassium carbonate (K2CO3, 2 eq.) were slowly added. The resultant mixture was then heated at reflux for 8 hours, after which the volatiles were removed, and the residue was partitioned between EtOAc and water. The EtOAc layer was washed with brine and dried over MgSO4. Evaporation of EtOAc gave 2-(4-(3,5-bis(hydroxymethyl)phenoxy)butyl)isoindoline-1,3-dione (13 g, 78% yield).

WORKUP

后处理

  1. temperatureat reflux for 8 hours
  2. customafter which the volatiles were removed
  3. customthe residue was partitioned between EtOAc and water
  4. washThe EtOAc layer was washed with brine
  5. dry with materialdried over MgSO4
  6. customEvaporation of EtOAc