HRID568654

反应详情

EQUATION

反应方程式

HRID 568654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

E-2'-fluoro-2-hydroxy-4-methoxy-3-methylbenzophenone O-acetyl oxime (22.0 g) is dissolved in 100 ml of DMF and added to a suspension of 2.5 g NaH in 100 ml DMF. An ice bath is applied to keep the reaction temperature >30° C. After 40 minutes the reaction is poured into H2O and extracted with ether. After washing well with H2O, the ether is dried and evaporated to give a crystalline product that is washed with cold hexane to give 3-(2-fluorophenyl)-6-methoxy-7-methyl-1,2-benzisoxazole, mp 105°-108° C.

WORKUP

后处理

  1. customAn ice bath is applied
  2. customthe reaction temperature >30° C
  3. extractionextracted with ether
  4. washAfter washing well with H2O
  5. dry with materialthe ether is dried
  6. customevaporated
  7. customto give a crystalline product that
  8. washis washed with cold hexane