反应 #344042

ord-066e3c7255f948169203a77cfb24a679

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他This compound was prepared
  2. 2
    其他to 3 days
  3. 3
    其他Chromatography of the crude product over the 40-fold amount of silica gel using 10% (V/V) of ethyl acetate in methylene chloride followed by crystallization from ether/hexane and recrystallization from ethyl acetate/hexane
  4. 4
    其他gave off-white crystals with m.p. 168°-169°

实验过程

This compound was prepared by reacting rac-3,4-dihydro-2-ethynyl-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol with 2-bromo-3-hydroxypyridine under the conditions described in Example 26, but using twice as much triethylamine and lengthening the reaction time to 3 days. Chromatography of the crude product over the 40-fold amount of silica gel using 10% (V/V) of ethyl acetate in methylene chloride followed by crystallization from ether/hexane and recrystallization from ethyl acetate/hexane gave off-white crystals with m.p. 168°-169°.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05260294uspto-grants-1993_11