HRID453123

反应详情

EQUATION

反应方程式

HRID 453123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-((3-(2-(benzyloxy)-4-chlorophenyl)-1,2,4-thiadiazol-5-yl)methoxy)-2,6-difluorobenzamide (0.05 g, 0.10 mmol) in dichloromethane (5 ml) was added methanesulfonic acid (0.50 ml, excess) at room temperature under nitrogen atmosphere and allowed to stir at same temperature for 90 min. After the completion of the reaction (TLC monitoring), the solution was cooled to 0° C. and basified with saturated NaHCO3 solution (aqueous) followed by extraction with EtOAc (3×25 ml). The combined organics was dried over anhydrous Na2SO4, filtered and concentrated. The residue was washed with ether to get the desired product (0.012 g, 30%).

WORKUP

后处理

  1. customAfter the completion of the reaction (TLC monitoring)
  2. extractionfollowed by extraction with EtOAc (3×25 ml)
  3. dry with materialThe combined organics was dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. washThe residue was washed with ether