HRID523039

反应详情

EQUATION

反应方程式

HRID 523039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

93.9 g (259 mmol) of 3-bromo-8,8-dimethyl-8H-indolo[3,2,1-de]acridine are dissolved in 1500 ml of dry THF. 135 ml (337 mmol) of a 2.5 M solution of n-butyllithium in cyclohexane are added dropwise at −70° C., and, after 1 h, 37 ml of trimethyl borate (336 mmol) are added dropwise. The mixture is allowed to come to room temperature over the course of 1 h, and the solvent is removed. The residue, which is uniform according to 1H-NMR, is employed in the subsequent reaction without further purification. The yield is 77 g (235 mmol), corresponding to 91% of theory.

WORKUP

后处理

  1. customto come to room temperature over the course of 1 h
  2. customthe solvent is removed
  3. customis employed in the subsequent reaction without further purification