反应详情

A mixture of 1.1 g (3.8 mmol) of 2-phenylbenzo[b]thiophen-3-ylsulfonylamide, 1.0 g (3.8 mmol) of N-(4-methoxy-6-methylpyrimidin-2-yl)phenylcarbamate, 0.6 g (4 mmol) of 1.8-diazabicyclo[5.4.0]undec-7-ene and 15 ml of dioxane is stirred for 4 hours at 20°-25° C. The reaction mixture is then taken up in 100 ml of water, acidified to pH 3 by adding 2N hydrochloric acid dropwise and then extracted with 3×30 ml of ethyl acetate. The combined extracts are dried and concentrated by evaporation. The residue is crystallised from ether, affording 1.35 g (78% of theory) of N-(2-phenylbenzo[b]thiophen-3-ylsulfonyl)-N'-(4-methoxy-6-methylprimidin-2-yl)urea with a melting point of 199°-202° C.

1. extractionextracted with 3×30 ml of ethyl acetate
2. customThe combined extracts are dried
3. concentrationconcentrated by evaporation
4. customThe residue is crystallised from ether