反应详情

Putting 63.7 g (300 mM) of 3,4-dichlorobenzylamine hydrochloride and 30.9 g (1.1 eq.) of sodium dicyanamide in 950 ml (15 V) of acetonitrile, the mixture was heated and refluxed for 3.5 hours. Distilling away the solvent, 600 ml of water was added to the residue (white solid) to disperse and wash. Obtained crystals were filtered off, and dispersed and washed in 600 ml of dichloromethane. Since residue of amine was recognized, the crystals were dispersed and washed again in 600 ml of water and 500 ml of dichloromethane. Crystals were filtered off, and dried overnight at 60° C., and 57.7 g (78.9%) of the captioned compound was obtained.

1. temperaturethe mixture was heated
2. temperaturerefluxed for 3.5 hours
3. distillationDistilling away the solvent, 600 ml of water
4. additionwas added to the residue (white solid)
5. additionto disperse
6. washwash
7. customObtained crystals
8. filtrationwere filtered off
9. additiondispersed
10. washwashed in 600 ml of dichloromethane
11. additionthe crystals were dispersed
12. washwashed again in 600 ml of water
13. filtrationCrystals were filtered off
14. customdried overnight at 60° C.