HRID2368869

反应详情

EQUATION

反应方程式

HRID 2368869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (E)-S-phenyl 3-(4-(methoxymethoxy)-3,5-dimethylstyryl)benzothioate (80 mg, 0.198 mmol) in i-PrOH and THF (½ mL) was added 0.5 mL of concentrated HCl. The reaction mixture was stirred overnight (about 18 hours). After removal of solvent under reduced pressure, the residue was dissolved in EtOAc. The solution was washed with brine and dried with Na2SO4. The solution was filtered and concentrated. The compound was purified by column chromatography (9:1 Hexane:EtOAc) to afford (E)-S-phenyl 3-(4-hydroxy-3,5-dimethylstyryl)-benzothioate in quantitative yield. Azo-linked compounds of Formula I are prepared following usual syntheses for preparing aromatic or heteroaromatic azo compounds. A typical scheme is shown in Scheme 3.

WORKUP

后处理

  1. customAfter removal of solvent under reduced pressure
  2. dissolutionthe residue was dissolved in EtOAc
  3. washThe solution was washed with brine
  4. dry with materialdried with Na2SO4
  5. filtrationThe solution was filtered
  6. concentrationconcentrated
  7. customThe compound was purified by column chromatography (9:1 Hexane:EtOAc)