HRID1493737

反应详情

EQUATION

反应方程式

HRID 1493737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

55 ml (85 mmol) of a 1.55 molar solution of n-butyllithium in hexane were added dropwise to a solution of 7.52 g (40 mmol) of N-(3-methoxybenzyl)-imidazole and 4.65 g (40 mmol) of TMEDA in 90 ml of absolute THF at -70° C. The mixture was stirred for a further 20 minutes at -70° C., and a solution of 6.01 g (40 mmol) of adamantanone in 30 ml of absolute THF was then added dropwise at -70° C. in the course of about 10 minutes. The procedure was then continued as described in Example 100. The residue (13 g) from the CH2Cl2 extract was crystallized from acetonitrile. 7.5 g of pure 3-methoxyphenyl-(2-hydroxy-2-adamantyl)-1-imidazolylmethane of melting point 182° C. were obtained.

WORKUP

后处理

  1. extractionThe residue (13 g) from the CH2Cl2 extract
  2. customwas crystallized from acetonitrile