반응 #57503

반응 방정식

hexane ethyl acetate

1,2,4-triazole

2-(3,5-dichlorophenoxy)-N-(1-chloro-6-methylhept-4-yn-6-yl) butyramide

potassium carbonate

→

required product

2-(3,5-dichlorophenoxy)-N-(6-methyl-1-(1,2,4-triazol-1-yl)-hept-4-yn-6-yl) butyramide

용매

water

ethyl acetate

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도cooled to ambient temperature
2. 2
   추출extracted with ethyl acetate (three times)
3. 3
   세척washed with brine
4. 4
   건조dried over magnesium sulphate
5. 5
   기타then evaporated under reduced pressure
6. 6
   기타to give a yellow oil

실험 절차

To a stirred solution of 2-(3,5-dichlorophenoxy)-N-(1-chloro-6-methylhept-4-yn-6-yl) butyramide (0.59 g) in dry N,N-dimethylformamide (10 ml) containing anhydrous potassium carbonate (0.28 g) was added 1,2,4-triazole (0.10 g). The mixture was heated to 90° C. for 2.75 hours, cooled to ambient temperature, diluted with water and extracted with ethyl acetate (three times). The extracts were combined, washed with brine, dried over magnesium sulphate then evaporated under reduced pressure to give a yellow oil. The oil was fractionated by chromatography (silica; hexane/ethyl acetate, 2:1 by volume followed by ethyl acetate) to give the required product as a colourless oil, 0.16 g, 1H NMR (CDCl3) δ: 1.00-1.06(3H, t); 1.60(3H, s); 1.62(3H, s); 1.92-2.14(6H, m); 4.38-4.44(3H, m); 6.26(1H, s); 6.84(2H, s); 7.04(1H, s); 7.96(1H, s); 8.32(1H, s).

출처