反応 #549683

反応方程式

sulphur trioxide

4-(3-methyl-2-pyridyl)butylamine hydrobromide

bromine

→

4-(5-bromo-3-methyl-2-pyridyl)-butylamine

収率 46.1%

溶媒

1,1,2-trifluorotrichloroethane

1,1,2-trifluorotrichloroethane

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度under reflux for ca 16 hr
3. 3
   その他The solvent was removed by distillation
4. 4
   その他was removed by acetylation

実験手順

A solution of sulphur trioxide (150 ml) in 1,1,2-trifluorotrichloroethane (550 ml) was added over 30 min to a suspension of 4-(3-methyl-2-pyridyl)butylamine hydrobromide (14.2 g) [prepared by reacting 4-(3-methyl-2-pyridyl)butylamine with hydrobromic acid (0.89M)] in 1,1,2-trifluorotrichloroethane and to this mixture was added liquid bromine (5.56 g). The mixture was heated under reflux for ca 16 hr. The solvent was removed by distillation and unbrominated starting material was removed by acetylation as described in Example 1(b) to yield 4-(5-bromo-3-methyl-2-pyridyl)-butylamine (6.49 g) as an oil.

出典