HRID1457683

反应详情

EQUATION

反应方程式

HRID 1457683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a cooled (0° C.) solution of 1.0 g of 10,11-dihydrodibenz[b,f][1,4]oxazepine and 7 ml of triethylamine in 30 ml of CH2Cl2 under argon is added dropwise 2.0 g of [1,1'-biphenyl]-4-carbonyl chloride. The mixture is stirred at room temperature for 16 hours and diluted with 50 ml of CHCl3. The mixture is washed with 30 ml each of H2O, 2NHCl, H2O, saturated NaHCO3, H2O, and dried (Na2SO4). Solvent is removed under vacuum to give 1.6 g of a yellow solid, m.p. 93°-95° C; Mass spectrum (CI), 378(MH+).

WORKUP

后处理

  1. washThe mixture is washed with 30 ml each of H2O
  2. dry with material2NHCl, H2O, saturated NaHCO3, H2O, and dried (Na2SO4)
  3. customSolvent is removed under vacuum