反应详情

A mixture of 4-(2-aminophenylamino)-2-chloro-2′-methylbenzophenone (Compound 156, 1.2 g, 3.5 mmol), dimethylcarbamyl chloride (0.32 ml, 3.5 mmol) and potassium carbonate (1.0 g, 7 mmol) in N,N-dimethylformamide (20 ml) was stirred at room temperature for 16 hours. The reaction mixture was poured into water (100 ml) and was extracted with ethyl acetate (3×75 ml). The organic phase was dried (MgSO4), filtered and evaporated in vacuo to give the crude product. The crude product was purified by flash chromatography by using ethyl acetate/pentane mixtures from 1:9 to 1:1. Trituration with diethyl ether/pentane 1:1 afforded the pure title compound.

1. extractionwas extracted with ethyl acetate (3×75 ml)
2. dry with materialThe organic phase was dried (MgSO4)
3. filtrationfiltered
4. customevaporated in vacuo
5. customto give the crude product
6. customThe crude product was purified by flash chromatography