HRID1165513

反应详情

EQUATION

反应方程式

HRID 1165513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (1R*,2R*)-1,2,3,4-tetrahydro-1-(1H-imidazol-1-ylmethyl)-6-methoxy-2-(4-methoxyphenyl)naphthalene, (prepared as described in Example 1), in dichloromethane (20 ml) was stirred in an argon atmosphere and cooled in an acetone/solid carbon dioxide bath while a 1M solution of boron tribromide was added dropwise over 5 minutes. The mixture was kept at -20° for 48 h, then poured into a mixture of saturated sodium bicaronate solution (30 ml) and stirred vigorously for 2 h. The solid thus obtained was filtered off, washed with water (100 ml) then dichloromethane (100 ml) and dried in a desiccator under reduced pressure to give (1R*,2R*)-1,2,3,4-tetrahydro-6-hydroxy-2-(4-hydroxyphenyl)-1-(1H-imidazol-1-ylmethyl)naphthalene, m.p. 238°.

WORKUP

后处理

  1. additionwas added dropwise over 5 minutes
  2. customThe solid thus obtained
  3. filtrationwas filtered off
  4. washwashed with water (100 ml)
  5. dry with materialdichloromethane (100 ml) and dried in a desiccator under reduced pressure