反应详情

温度

60 °C

A stirred suspension of 7,8-dihydroimidazo[1,5-c]pyrimidin-5(6H)-one (699.7 g) in DMF 2.45 litres) was heated to ca. 60° C. A solution of methyl 4-methylbenzenesulfonate (1058.2 g.) in DMF (0.7 litres) was added over 100 min at ca. 60° C., and rinsed in with DMF (0.35 litres). The white suspension was stirred at ca. 60° C. for 200 min. when the reaction was complete by nmr. The reaction mixture was allowed to cool to ca. 40° C. and TBME (5.25 litres) was added. The product was cooled to ca. 22° C., aged at this temperature for 17 h, and filtered. The cake was washed with TBME-DMF (3:1, 1.4 litres), then with TBME (2×1.4 litres), the cake was pulled dry, and the product was dried in vacuo at ca. 50° C. to yield the title compound, 1583.5 g.

1. washrinsed in with DMF (0.35 litres)
2. temperatureto cool to ca. 40° C.
3. additionTBME (5.25 litres) was added
4. temperatureThe product was cooled to ca. 22° C.
5. waitaged at this temperature for 17 h
6. filtrationfiltered
7. washThe cake was washed with TBME-DMF (3:1, 1.4 litres)
8. dry with materialwith TBME (2×1.4 litres), the cake was pulled dry
9. customthe product was dried in vacuo at ca. 50° C.