反应详情

温度

20 °C

1.7 g of methylamine hydrochloride was added to 5.2 g (23 mmol) of α-(2-methoxymethylphenyl)-β-methylacrylic chloride in 30 ml of dichloromethane, and 4 g of pyridine was dripped in at 0° to 5° C. The mixture was stirred for a further 15 hours at about 20° C. The reaction mixture was diluted with 20 ml of dichloromethane and washed with water. The organic phase was dried over sodium sulfate and evaporated down. The crude product was chromatographed on silica gel with methyl tert-butyl ether/cyclohexane (5/1). Removal of the solvent gave 1.5 g (30%) of the title compound in the form of colorless crystals (m.p.: 58° C.).

1. customwas dripped in at 0° to 5° C
2. washwashed with water
3. dry with materialThe organic phase was dried over sodium sulfate
4. customevaporated down
5. customThe crude product was chromatographed on silica gel with methyl tert-butyl ether/cyclohexane (5/1)
6. customRemoval of the solvent