反应详情

A mixture of 7.4 g of N1 -[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl]-1,2-ethanediamine, 4.1 g 2-chloropyrimidine, 4.2 g of sodium carbonate and 50.6 ml of ethanol was stirred for 4 hours at reflux temperature. The reaction mixture was evaporated. The residue was purified by column chromatography (silica gel; CHCl3 /CH3OH 90:10). The eluent of the desired fraction was evaporated and the residue was converted into the hydrochloride salt in 2-propanol. The salt was filtered off and dried in vacuo, yielding 4.4 g (33.3%) of (±)-N-[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl]-N'-(2-pyrimidinyl)-1,2-ethanediamine dihydrochloride hemihydrate; mp. 192.7° C. (comp. 1).

1. temperatureat reflux temperature
2. customThe reaction mixture was evaporated
3. customThe residue was purified by column chromatography (silica gel; CHCl3 /CH3OH 90:10)
4. customThe eluent of the desired fraction was evaporated
5. filtrationThe salt was filtered off
6. customdried in vacuo