反応 #64884

反応方程式

methylamine hydrochloride

α-(2-methoxymethylphenyl)-β-methylacrylic chloride

pyridine

→

title compound

収率 30.0%

α-(2-methoxymethylphenyl)-β-methylacrylic acid-N-methylamide

収率 30.0%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   その他was dripped in at 0° to 5° C
2. 2
   洗浄washed with water
3. 3
   乾燥The organic phase was dried over sodium sulfate
4. 4
   その他evaporated down
5. 5
   その他The crude product was chromatographed on silica gel with methyl tert-butyl ether/cyclohexane (5/1)
6. 6
   その他Removal of the solvent

実験手順

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.).

出典