HRID2220201
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
To a mixture of 8-Bromo-2-chloro-5,6,11,12-tetrahydro-dibenzo[b,f]azocine-12-ol (0.85 g, 2.5 mmole) in dioxane (10 mL) was added concentrated HCl (1 mL). The reaction was heated to reflux for 24 hours. The reaction mixture was concentrated and the residue obtained was dissolved in ethyl acetate, washed with saturated aqueous NaHCO3, dried (Na2SO4), filtered and concentrated to give 8-Bromo-2-chloro-5,6-dihydro-dibenzo[b,f]azocine (0.7 g, 87%). HPLC Rt=4.33 min. m/z=320 (M+H+).
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureto reflux for 24 hours
- concentrationThe reaction mixture was concentrated
- customthe residue obtained
- washwashed with saturated aqueous NaHCO3
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated