반응 #64884
ord-89088b4bbe7645989ca3c608b470a08e
반응 방정식
반응 조건
온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타was dripped in at 0° to 5° C
- 2세척washed with water
- 3건조The organic phase was dried over sodium sulfate
- 4기타evaporated down
- 5기타The crude product was chromatographed on silica gel with methyl tert-butyl ether/cyclohexane (5/1)
- 6기타Removal of the solvent
실험 절차
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.).