HRID1771128

反应详情

EQUATION

反应方程式

HRID 1771128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a solution of N-(4-fluoro-3-(quinoxaline-6-carbonyl)phenyl)pivalamide (495 mg, 1.35 mmol, 1.0 eq.) in HOAc (10 mL) was added conc. HCl (8 mL). The mixture was stirred at 110° C. for 4 h, then poured onto ice. The mixture was basified to pH 10 by the addition of aqueous NaOH (1 N) and extracted with DCM (20 mL×3). The combined organic layers were dried over Na2SO4 and concentrated. The resulting residue was purified via flash column chromatography (PE/EA=½, v/v) to afford (5-amino-2-fluorophenyl)(quinoxalin-6-yl)methanone (380 mg, 99%).

WORKUP

后处理

  1. additionpoured onto ice
  2. extractionextracted with DCM (20 mL×3)
  3. dry with materialThe combined organic layers were dried over Na2SO4
  4. concentrationconcentrated
  5. customThe resulting residue was purified via flash column chromatography (PE/EA=½, v/v)