反应详情

温度

90 °C

A mixture of 2-methyl-5-oxo-5,6,7,8-tetrahydroimidazo[1,5-c]pyrimidin-2-ium 4-methylbenzenesulfonate (625.1 g), 4-methylbenzenesulfonic acid hydrate (406.6 g), 1,4-dioxan (9.38 litres) and water (625 ml) was heated at reflux (ca. 90° C.) for 2.5 h. when the reaction was complete by nmr. The reaction mixture was concentrated by distillation at atmospheric pressure collecting 7.03 litres. The concentrate was allowed to cool to ca. 77° C., and IMS-G (1.56 litres) was added. The resulting bright solution was allowed to cool and was seeded with [2-(1-methyl-1H-imidazol-4-yl)ethyl]amine bis(4-methylbenzenesulfonate) (0.625 g) at ca. 54° C. The suspension was allowed to cool to ca. 22° C. and aged for 40 min. The solid was filtered off and washed successively with 1,4-dioxan-IMS (3:1, 1.25 litres), and then 1,4-dioxan (2×1.25 litres), pulled dry and dried in vacuo at ca. 50° C. to yield the title compound, 866.3 g.

1. temperaturewas heated
2. concentrationThe reaction mixture was concentrated by distillation at atmospheric pressure
3. customcollecting 7.03 litres
4. temperatureto cool to ca. 77° C.
5. additionIMS-G (1.56 litres) was added
6. temperatureto cool
7. customwas seeded with [2-(1-methyl-1H-imidazol-4-yl)ethyl]amine bis(4-methylbenzenesulfonate) (0.625 g) at ca. 54° C
8. temperatureto cool to ca. 22° C. and aged for 40 min
9. filtrationThe solid was filtered off
10. washwashed successively with 1,4-dioxan-IMS (3:1, 1.25 litres)
11. dry with material1,4-dioxan (2×1.25 litres), pulled dry
12. customdried in vacuo at ca. 50° C.