HRID3932

反应详情

EQUATION

反应方程式

HRID 3932 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20 ml of a 30% aqueous solution of sodium hydroxide was added dropwise to a mixture of 2 g (0.007 mol) of 2-(p-hydroxyphenyl)-5-octylpyridine and 1.65 g (0.007 mol) of (R)-1-bromo-(4-methyl)decane with stirring. The resulting solution was heated to a temperature between about 90° and 100° C. for 3 hours. 150 ml of water was added to the reaction solution and the organic layer was extracted with chloroform. After washing the extract three times with water, chloroform was removed by distillation. The residue was chromatographed over 2.5×100 (cm) of silica gel and developed with hexane and benzene. The effluent was repeatedly recrystallized from a mixture of methanol and acetone to yield 1.44 g (0.0033 mol) of (R)2-[p-(4-methyldecyloxy)phenyl]-5-octylpyridine.

WORKUP

后处理

  1. temperatureThe resulting solution was heated to a temperature between about 90° and 100° C. for 3 hours
  2. extractionthe organic layer was extracted with chloroform
  3. washAfter washing the
  4. extractionextract three times with water, chloroform
  5. customwas removed by distillation
  6. customThe residue was chromatographed over 2.5×100 (cm) of silica gel
  7. customThe effluent was repeatedly recrystallized from a mixture of methanol and acetone