反应详情

温度

22 °C

Carbonyldiimidazole (970.2 g) was added to a stirred suspension of [2-(1-methyl-1H-imidazol-4-yl)ethyl]amine dihydrochloride (999.9 g) (commercial eg Sigma) and imidazole (37 g) in dichloromethane (5.3 litres) at ca 22° C. The resulting white suspension was heated at reflux until reaction was complete by nmr (4 h.). Solvent (8 litres) was distilled off at atmospheric pressure whilst adding IMS-G (8 litres). Additional IMS-G (2 litres) was added and the suspension cooled to ca. 22° C. and aged at this temperature for at 2 h. The solid was collected by filtration, washed with IMS-G (2×0.5 litres), pulled dry and dried in vacuo at ca. 60° C. to yield the title compound, 478 g.

1. temperatureThe resulting white suspension was heated
2. temperatureat reflux until reaction
3. customwas complete by nmr (4 h.)
4. distillationSolvent (8 litres) was distilled off at atmospheric pressure
5. additionwhilst adding IMS-G (8 litres)
6. additionAdditional IMS-G (2 litres) was added
7. customaged at this temperature for at 2 h
8. filtrationThe solid was collected by filtration
9. washwashed with IMS-G (2×0.5 litres)
10. custompulled dry
11. customdried in vacuo at ca. 60° C.