HRID2234451

反应详情

EQUATION

反应方程式

HRID 2234451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Amino-2-fluorobenzoic acid tert-butyl ester (ABChem. Inc.; 1 g, 4.73 mmol) in DMF (15 mL) was added dropwise to N-chlorosuccinimide (633 mg, 4.73 mmol) in DMF (20 mL). The mixture was stirred at room temperature for 72 hours. The reaction mixture was poured into water (130 mL) and extracted with ethyl acetate (2×50 mL). The combined extracts were washed with water, brine, dried (MgSO4) and concentrated. Column chromatography (5% ethyl acetate/isohexane) yielded the title compound as a pale yellow, crystalline solid (321 mg, 27.5%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (2×50 mL)
  2. washThe combined extracts were washed with water, brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated