反应详情

温度

70 °C

A mixture of 6.7 g of 1,1′-(4-iodobutylidene)bis[4-fluorobenzene], 5.2 g of 3-[(methylamino)carbonyl]-N-(2,4,6-trimethylphenyl)-1-piperazineacetamide, 2.3 g sodium carbonate and 38 ml DMF is stirred for 18 hours at 70° C. The reaction mixture is cooled and poured onto ice-water. The product is extracted with DCM. The extract is washed with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is dried, yielding 4.23 g of 4-[4,4-bis(4-fluorophenyl)butyl]-3-[(methylamino)-carbonyl]-N-(2,4,6-trimethylphenyl)-1-piperazineacetamide (compound 1, mp. 82.3° C.).

1. temperatureThe reaction mixture is cooled
2. additionpoured onto ice-water
3. extractionThe product is extracted with DCM
4. washThe extract is washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe residue is purified by column-chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
10. customThe pure fractions are collected
11. customthe eluent is evaporated
12. customThe residue is dried