HRID1925361

反应详情

EQUATION

反应方程式

HRID 1925361 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

To a stirred solution of methyl 6-hydroxy-1-naphthoate (25 g, 123.8 mmol) in anhydrous acetonitrile (130 mL), SelectFluor (45 g, 127.5 mmol) was added and the reaction vessel sealed (sealed tube). The reaction mixture was heated to 85° C. for 3 d. The reaction mixture was allowed to cool to RT, diluted with ethyl acetate and washed with water, then brine, dried with Na2SO4, filtered and evaporated. The mixture was purified by column chromatography using methylene chloride as the eluent. The title compound was obtained as a tan solid.

WORKUP

后处理

  1. customthe reaction vessel sealed
  2. custom(sealed tube)
  3. temperatureto cool to RT
  4. washwashed with water
  5. dry with materialbrine, dried with Na2SO4
  6. filtrationfiltered
  7. customevaporated
  8. customThe mixture was purified by column chromatography