HRID561455

反应详情

EQUATION

反应方程式

HRID 561455 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

16.5 ml (26.5 mmol) of a 1.6N solution of n-butyllithium in hexane were added dropwise to a solution of 5.00 g (26.5 mmol) of 4-bromo-3-fluorotoluene in 40 ml of THF at −78° C., and the mixture was stirred for 0.5 h. Then, at −78° C., a solution of 2.72 g (17.6 mmol) of the compound from Example 73A in 10 ml of THF was added, and the mixture was allowed to warm to RT and was stirred at RT for 2 h. Water was added, the mixture was concentrated, and the crude product was purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% formic acid). 300 mg (9% of theory) of the title compound were obtained.

WORKUP

后处理

  1. stirringwas stirred at RT for 2 h
  2. concentrationthe mixture was concentrated
  3. customthe crude product was purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with addition of 0.1% formic acid)