HRID388364
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
1,2,4-triazole (248 mg) is added to a solution of 4-fluoro-naphthalene-1-carbaldehyde (522 mg) and potassium carbonate (4 mg) in DMF (4 ml): After 3 hours a room temperature, the reaction is quenched with water (40 ml) and ethyl acetate (50 ml). The organic phase is separated and the aqueous phase is extracted two times with ethyl acetate. The organic phases are combined, extracted with water and with a saturated aqueous solution of NaCl, dried over Na2SO4 and concentrated in vacuo. The crude product is purified on a semi-preparative HPLC to yield 4-[1,2,4]triazol-1-yl-naphthalene-1-carbaldehyde (460 mg) as beige crystals. MS (HPLC/MS): 224 (MH+). Retention time: 2.97 min.
WORKUP
后处理
- customthe reaction is quenched with water (40 ml) and ethyl acetate (50 ml)
- customThe organic phase is separated
- extractionthe aqueous phase is extracted two times with ethyl acetate
- extractionextracted with water and with a saturated aqueous solution of NaCl
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customThe crude product is purified on a semi-preparative HPLC