HRID2220201

反应详情

EQUATION

反应方程式

HRID 2220201 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 24 hours
  3. concentrationThe reaction mixture was concentrated
  4. customthe residue obtained
  5. washwashed with saturated aqueous NaHCO3
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated