反应详情

温度

160 °C

A mixture of 3.97 ml (52 mmol, 10 eq) allylamine, 0.97 g (5.2 mmol, 1 eq) 2-chloro-6-methoxy-isonicotinic acid (see building block A3) and 1.29 g (5.2 mmol, 1 eq)-copper(II) sulfate pentahydrate in 10 ml water is heated in a closed vessel during 2.5 h at a bath temperature of 160° C. After cooling to rt the mixture is diluted with 400 ml aq 10% citric acid and extracted with EtOAc. The extracts are washed with water and brine, dried over sodium sulfate and the solvents are evaporated at reduced pressure. The residue is dissolved in about 20 ml hot DCM/MeOH (2/1). On addition of about 25 ml of hexane, partial evaporation of the solvents to a volume of about 20 ml and keeping at 4° C. for 4 h the product precipitates and is filtered off and dried in vacuum.

1. temperatureAfter cooling to rt the mixture
2. extractionextracted with EtOAc
3. washThe extracts are washed with water and brine
4. dry with materialdried over sodium sulfate
5. customthe solvents are evaporated at reduced pressure
6. dissolutionThe residue is dissolved in about 20 ml hot DCM/MeOH (2/1)
7. additionOn addition of about 25 ml of hexane, partial evaporation of the solvents to a volume of about 20 ml
8. customthe product precipitates
9. filtrationis filtered off
10. customdried in vacuum