HRID342765

反应详情

EQUATION

反应方程式

HRID 342765 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 methyl 3-chloro-4-(3-(3-phenyl-7-propylbenzofuran-6-yloxy)propylthio)-phenylacetate (3.72 g, 7.31 mmol) prepared in last step and aqueous lithium hydroxide(1.0M; 14.62 ml; 14.62 mmol) in methanol (25 ml) was refluxed for 1 hr. The mixture was partitioned between isopropyl acetate and pH4 buffer. The organic was dried over sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by chromatography (silica gel, 50% methylene chloride in hexane) to afford the title compound. M.P: 143° C. ESI-MS: m/e-495(M+1)

WORKUP

后处理

  1. temperaturewas refluxed for 1 hr
  2. customThe mixture was partitioned between isopropyl acetate and pH4 buffer
  3. dry with materialThe organic was dried over sodium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by chromatography (silica gel, 50% methylene chloride in hexane)