反应详情

To a stirred solution of pyridine-2-carboxylic acid methoxy-methyl-amide (10.0 g, 0.060 mol) in anhydrous THF (150 mL) at −78° C. was added freshly prepared Grignard reagent of 4-bromo anisole (20.0 g, 0.106 mol). The reaction mixture was allowed to warm to room temperature. Reaction mixture was quenched with saturated ammonium chloride (100 mL) and extracted with ethyl acetate (2×200 mL). Organic layer was dried over sodium sulphate and concentrated. Purification by 100-200-mesh sized silica gel column with 0-20% EtoAc:Hexane as eluent provided the product.

1. customReaction mixture
2. customwas quenched with saturated ammonium chloride (100 mL)
3. extractionextracted with ethyl acetate (2×200 mL)
4. dry with materialOrganic layer was dried over sodium sulphate
5. concentrationconcentrated
6. customPurification by 100-200-mesh sized silica gel column with 0-20% EtoAc
7. customHexane as eluent provided the product