HRID49642

反应详情

EQUATION

反应方程式

HRID 49642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
220 °C

PROCEDURE

实验过程

A mixture of 7-(2-naphthoyl)-3-methyl-5,6-dihydro-2(4H)-benzofuranone (10 g) and acetic acid potassium salt (0.3 g) was added to a reactor and stirred for 1 hr at 220° C. The reaction mixture was cooled down to room temperature. Toluene and water were added to the reaction mixture and acidified to pH 2 with 5% hydrochloric acid. Toluene layer separated was dried over anhydrous MgSO4, filtered and evaporated to give crude product. The crude product was purified by column chromatograph on silica gel by eluting with a mixture of ethylacetate and n-hexane (1:5) to give the desired product (9:42 g, 94 % .

WORKUP

后处理

  1. additionwas added to a reactor
  2. temperatureThe reaction mixture was cooled down to room temperature
  3. customToluene layer separated
  4. dry with materialwas dried over anhydrous MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customto give crude product
  8. customThe crude product was purified by column chromatograph on silica gel
  9. washby eluting with a mixture of ethylacetate and n-hexane (1:5)