反应详情

5.0 g (3.54 mmol) of 1-fluoro-3-nitrotoluene, 9.89 g (5.31 mmol) of tert-butyl 1-piperazinecarboxylate and 27.0 g (19.5 mmol) of potassium carbonate are solubilized under an argon atmosphere in DMSO (60 ml), then the reaction medium is taken to 100° C. for 72 hours. The reaction medium is then cooled down using an ice bath then poured into ice-cold water. The product is extracted using 3 times 50 ml of dichloromethane. The organic solution is dried over magnesium sulphate, followed by filtration and concentration under vacuum. Purification on a silica column is then carried out (eluent=heptane 70%/ethyl acetate 30%) in order to produce a yellow solid. The yellow solid is further purified by recrystallization from diisopropyl ether in order to produce 4.5 g of the expected product (yield 42.0%). Melting point: 82.0-92.0° C.

1. temperatureThe reaction medium is then cooled down
2. additionthen poured into ice-cold water
3. extractionThe product is extracted
4. dry with materialThe organic solution is dried over magnesium sulphate
5. filtrationfollowed by filtration and concentration under vacuum
6. customPurification on a silica column
7. customto produce a yellow solid
8. customThe yellow solid is further purified by recrystallization from diisopropyl ether in order