HRID500514

反应详情

EQUATION

反应方程式

HRID 500514 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To solution of 2-fluoro-4-iodoaniline (9.21 g, 38.86 mmol) and 3,6-Dichloro-pyridazine-4-carboxylic acid (10.84 g, 64.77 mmol) in THF (80 mL) at −78° C., was added LiHMDS (5 g, 25.91 mmol). The mixture was allowed to warm to room temperature and stirred for 12 h. The mixture as diluted with ethyl acetate and washed with H2O and brine. The organic layer was dried with solid Na2SO4 and was concentrated. The resulting residue was purified by flash chromatography in silica (25% ethyl acetate-hexane) to give pure product. LC/MS [4.52 min; 394 (M+1)].

WORKUP

后处理

  1. washwashed with H2O and brine
  2. dry with materialThe organic layer was dried with solid Na2SO4
  3. concentrationwas concentrated
  4. customThe resulting residue was purified by flash chromatography in silica (25% ethyl acetate-hexane)
  5. customto give pure product
  6. customLC/MS [4.52 min; 394 (M+1)]