反应详情

Under a protective gas, 27.07 g of 2-(5-amino-4-ethoxycarbonyl-1H-pyrrol-2-yl)-N-benzyl-pyridinium bromide in 195 ml of formamide are heated for 16 hours at 150° C. with 97.6 ml of DMF (dried over 4A molecular sieve) and 48.8 ml of formic acid. When the dark-brown reaction mixture is cooled in an ice-bath, the title compound crystallizes and can be filtered off and washed with isopropanol and diethyl ether; 1H-NMR (300 MHz, DMSO-d6): 12.5 and 11.9 (2s, 2H), 8.60 (d, J=7, 1H), 8.05-7.8 (m, 3H), 7.28 (dd, J1 =7, J2 =9, 1H), 7.20 (s, 1H); FAB-MS: (M+H)+ =213.

1. temperatureWhen the dark-brown reaction mixture is cooled in an ice-bath
2. customthe title compound crystallizes
3. filtrationcan be filtered off
4. washwashed with isopropanol and diethyl ether