反应详情

温度

0 °C

[3,5-Bis-(4-cyano-phenoxy)-phenyl]-amine (0.35 g, 1.07 mmol) and 2-naphthyl-sulphonyl chloride (0.29 g, 1.28 mmol) were dissolved in 10 ml of dichloromethane and cooled to 0° C. Further 0.18 ml (2.14 mmol) of pyridine and 15 mg (0.107 mmol) of DMAP was added to the reaction mixture and allowed to stirred overnight at RT. After completion, reaction mixture was diluted with 50 ml of dichloromethane and washed with 50 ml 1N HCl solution and then with brine. Organic layer was dried over anhydrous sodium sulphate and concentrated under vacuo. Thus obtained crude product was subjected to column chromatography and eluted with ethylacetate and hexane mixture to afford 0.4 g of the required product. Percentage purity (LCMS): 90.4% M+1=517.1+1.

1. customAfter completion, reaction mixture
2. washwashed with 50 ml 1N HCl solution
3. dry with materialOrganic layer was dried over anhydrous sodium sulphate
4. concentrationconcentrated under vacuo
5. customThus obtained crude product
6. washeluted with ethylacetate and hexane mixture