反应详情

温度

20 °C

A reactor was charged at about 20° C. with the compound of formula (I) form A0 (6.075 kg; 1 eq) and dichloromethane (92 L; 15 V). The mixture was stirred (80 rpm) at 20° C. for 15 minutes. After cooling the mixture to 10° C., paratoluene sulfonic acid (PTSA—2.417 kg; 1 eq) was added portion wise. The mixture was stirred at 80 rpm at 10° C. for 1 hour. Then, MTBE (122 L; 15 V) was added portion wise via a feed vessel. The mixture was heated to 45° C. at least 1 h (checking that the reaction was complete by RX/DSC, if it is necessary, continue the contact). After cooling the mixture to 10° C., the precipitated solids were isolated by filtration and washed with MTBE. The product was dried under vacuum at 40° C. to yield the addition salt of compound of formula (I) with PTSA (8.045 kg; yield=97.3%; purity=99.1%).

1. temperatureAfter cooling the mixture to 10° C.
2. stirringThe mixture was stirred at 80 rpm at 10° C. for 1 hour
3. temperatureThe mixture was heated to 45° C. at least 1 h (checking that the reaction
4. temperatureAfter cooling the mixture to 10° C.
5. customthe precipitated solids were isolated by filtration
6. washwashed with MTBE
7. customThe product was dried under vacuum at 40° C.