HRID388364

反应详情

EQUATION

反应方程式

HRID 388364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customthe reaction is quenched with water (40 ml) and ethyl acetate (50 ml)
  2. customThe organic phase is separated
  3. extractionthe aqueous phase is extracted two times with ethyl acetate
  4. extractionextracted with water and with a saturated aqueous solution of NaCl
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe crude product is purified on a semi-preparative HPLC