HRID454862

反应详情

EQUATION

反应方程式

HRID 454862 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 6-bromophthalazin-1-ol (1.00 g, 4.44 mmol), 4-fluorobenzenamine (0.642 g, 5.78 mmol), Pd(dppf)Cl2.CH2Cl2 (0.130 g, 0.178 mmol), and lithium bis(trimethylsilyl)amide (2.23 g, 13.3 mmol) in 2-methyltetrahydrofuran (10 mL) was heated at 95° C. in an oil bath for 24 h in a sealed tube. The mixture was cooled to RT, diluted with MeOH and filtered through a pad of Celite. The filtrate was concentrated over silica gel. The residue was purified using column chromatography (0-4% MeOH in CH2Cl2) to yield the title compound as a yellow crystalline solid. MS (ESI, pos. ion) m/z: 256.0 (M+1).

WORKUP

后处理

  1. filtrationfiltered through a pad of Celite
  2. concentrationThe filtrate was concentrated over silica gel
  3. customThe residue was purified