HRID1094504
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
48 μl (0.68 mMol) acetyl chloride are added portionwise to a solution of 300 mg (0.68 mMol) 6-(2-amino-pyrimidin-4-yloxy)-naphthalene-1-carboxylic acid (4-fluoro-3-trifluoromethyl-phenyl)-amide (step 10.3) in 3.7 ml CH2Cl2 and 5.5 ml pyridine. After 1.5 h, the solution is diluted with EtOAc and water, the aq. phase separated off and extracted twice with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Chromatography (Combi Flash; hexane/EtOAc 1:1→1:3) gives the title compound: m.p.: 213-214° C.
WORKUP
后处理
- customthe aq. phase separated off
- extractionextracted twice with EtOAc
- washThe organic layers are washed with water and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated