HRID2384880

反应详情

EQUATION

反应方程式

HRID 2384880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine toluene-4-sulfonic acid 2-methoxy-4-[2-(4-methoxy-phenyl)-7-oxo-4,7-dihydro-5H-thieno[2,3-c]pyridin-6-yl]-phenyl ester (1.029 g, 1.92 mmol) and KOH (2.15 g, 38.48 mmol) with EtOH (30 mL) and water (20 mL). Reflux the reaction for 10 h and dilute with water (50 mL). Acidify with 5.0 M HCl (8 mL). Remove the organic solvent in vacuo and dilute the residue with water (10 mL). Collect the solid material by filtration and wash with water (3×10 mL) and Et2O (2×15 mL) then dry in a vacuum oven to give 0.646 g (88%) of the title compound. MS/ES m/z 382.0 [M+H]+.

WORKUP

后处理

  1. temperatureReflux
  2. customthe reaction for 10 h
  3. customRemove the organic solvent in vacuo
  4. additiondilute the residue with water (10 mL)
  5. customCollect the solid material
  6. filtrationby filtration
  7. washwash with water (3×10 mL) and Et2O (2×15 mL)
  8. customthen dry in a vacuum oven