HRID745990

反应详情

EQUATION

反应方程式

HRID 745990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.8 g (7.33 mmol) of [[5-bromo-3-(2-fluorophenyl)-1,2-benzisoxazol-6-yl]thio]acetic acid was combined with 30 ml (2 eq.) of 0.5M sodium periodate solution in 300 ml of 4:1 methanol/water. The mixture was refluxed for 18 hours during which the insoluble sodium iodate precipitated. The reaction mixture was then poured into excess 3N HCl and extracted several times with ethyl acetate. The ethyl acetate extracts were combined, washed with water and a saturated salt solution, dried over magnesium sulfate, filtered and evaporated to yield a white solid. The solid was triturated with hexanes and dried under vacuum to yield 2.51 g (86%) of [[5-bromo-3-(2-fluorophenyl)-1,2-benzisoxazol-6-yl]sulfinyl]acetic acid, m.p. 173°-174° C.

WORKUP

后处理

  1. customprecipitated
  2. additionThe reaction mixture was then poured into excess 3N HCl
  3. extractionextracted several times with ethyl acetate
  4. washwashed with water
  5. dry with materiala saturated salt solution, dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto yield a white solid
  9. customThe solid was triturated with hexanes
  10. customdried under vacuum