HRID440621

反应详情

EQUATION

反应方程式

HRID 440621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-naphthol (3.23 g;0.0224 mol), 1,1-dianisylprop-2-yn-1-ol (6.00 g;0.0224 mol), acidic alumina Brockmann 1(6 g) and toluene (250 ml) was heated and stirred for 1.5 h, cooled, filtered and the solid washed with toluene. The filtrate was evaporated to give a pale purple tacky solid which was washed with pet. ether (40-60)/diethyl ether to yield crude product (7.07 g). Purification of the solid by crystallisation from ethylacetate gave 3,3-dianisyl-3H-naphtho[2,1-b]pyran as a white solid (5.52 g;66% yield), m.pt 176°-177° C. ##STR10##

WORKUP

后处理

  1. temperaturewas heated
  2. temperaturecooled
  3. filtrationfiltered
  4. washthe solid washed with toluene
  5. customThe filtrate was evaporated
  6. customto give a pale purple tacky solid which
  7. washwas washed with pet. ether (40-60)/diethyl ether
  8. customto yield crude product (7.07 g)
  9. customPurification of the solid
  10. customby crystallisation from ethylacetate