HRID1494541

反应详情

EQUATION

反应方程式

HRID 1494541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1.6M n-butyl lithium in n-hexane (16.5 ml) in toluene (20 ml) at -20° C., under nitrogen, was added a solution of 2-bromo-6,7,8,9-tetrahydro-3-methyl-5H-cyclohepta[b]pyridine (6 g, 0.025 m) in toluene (30 ml) and kept at -20° C. for 0.25 hours. This was blown over into a solution of 3-pyridine carboxaldehyde (2.7 g) in toluene (30 ml) kept at -20° C. The solution was allowed to warm up to room temperature and water added. The organic phase was separated, dried (MgSO4) and evaporated. The solid was recrystallised from ether (twice) to give 1-(6,7,8,9-tetrahydro-3-methyl-5H-cyclohepta[b]pyrid-2-yl)-1-(pyrid-3-yl)methanol (4.32 g, 64%) m.p. 124°-6° C.

WORKUP

后处理

  1. customkept at -20° C
  2. customThe organic phase was separated
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customThe solid was recrystallised from ether (twice)