HRID597975
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
6-(3-Pyridinyl)-3-azabicyclo[3.2.1]oct-6-ene (190 mg, 1.0 mmol) was dissolved in ethanol (5 ml), and 12 N HCl (2 ml) was added. The solution was sonicated for 3 min, and then concentrated by azeotropic rotary evaporation with ethanol (3×5 ml) to yield a fluffy solid. Then the salt was dissolved in hot isopropanol (2 ml), and diethyl ether was added until a milky solution formed. Cooling in the freezer produced a light brown solid. The solid was filtered, washed with diethyl ether, and dried under high vacuum to yield 6-(3-pyridinyl)-3-azabicyclo[3.2.1]oct-6-ene dihydrochloride, (230 mg, 87%, m.p. 192-195° C.).
WORKUP
后处理
- customThe solution was sonicated for 3 min
- concentrationconcentrated by azeotropic rotary evaporation with ethanol (3×5 ml)
- customto yield a fluffy solid
- customformed
- temperatureCooling in the freezer
- customproduced a light brown solid
- filtrationThe solid was filtered
- washwashed with diethyl ether
- customdried under high vacuum