تفاعل #64884

معادلة التفاعل

methylamine hydrochloride

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

pyridine

→

title compound

المردود 30.0%

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

المردود 30.0%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىwas dripped in at 0° to 5° C
2. 2
   غسيلwashed with water
3. 3
   تجفيفThe organic phase was dried over sodium sulfate
4. 4
   أخرىevaporated down
5. 5
   أخرىThe crude product was chromatographed on silica gel with methyl tert-butyl ether/cyclohexane (5/1)
6. 6
   أخرىRemoval of the solvent

الإجراء التجريبي

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.).

المصدر