反应详情

温度

50 °C

Aluminium trichloride (112 g, 838 mmol) was suspended in dichloromethane (250 mL) at 0° C. A solution of N-(3,4-difluoro-2-methylbenzyl)-N-(2,2-dimethoxyethyl)-4-methylphenyl-sulphonylamine (42, 68.3 g) in dichloromethane (250 mL) was added. The reaction mixture was heated at 50° C. for 2 hours, before being cooled to 0° C. and poured on ice. The organic layer was separated, and the aqueous layer extracted twice more with dichloromethane/isopropanol (3:1). The combined organic phase was extracted twice with saturated sodium bicarbonate solution and dried over magnesium sulphate, before filtration and evaporation gave 63.5 g of crude dark brown semi-solid product. This was purified by chromatography on silica gel. Elution with ethyl acetate/heptane (5%:95% to 35%:65%) gave 11.3 g of the title compound 43 as a tan-coloured solid. Rt=0.86 min (Method 10). Detected mass: 180.1 (M+H+).

1. temperaturebefore being cooled to 0° C.
2. additionpoured on ice
3. customThe organic layer was separated
4. extractionthe aqueous layer extracted twice more with dichloromethane/isopropanol (3:1)
5. extractionThe combined organic phase was extracted twice with saturated sodium bicarbonate solution
6. dry with materialdried over magnesium sulphate, before filtration and evaporation
7. customgave 63.5 g of crude dark brown semi-solid product
8. customThis was purified by chromatography on silica gel
9. washElution with ethyl acetate/heptane (5%:95% to 35%:65%)