反应详情

温度

75 °C

Under argon gas atmosphere, a mixture of a solution of the compound prepared in Example 5 (177.6 g) in N,N-dimethylacetamide (355 mL) and a solution of triethylamine (103.2 g) and 3-aminopentane (88.9 g) in isopropyl alcohol (178 mL) was stirred for 4 hours at 95 to 105° C. of internal temperature. Water was poured into the reaction solution that was cooled to 70 to 80° C. of internal temperature. The diluted solution was cooled to 50 to 60° C. of internal temperature, and then after the crystal was precipitated, the solution was stirred for 30 minutes. Furthermore, water was poured into the solution, and the diluted solution was stirred for 1 hour at 20 to 30° C. of internal temperature. The precipitated crystal was collected by filtration, and the obtained crystal was dried under reduced pressure for 14 hours or more at about 50° C. to give the crude crystal of the title compound (174 g, (97.4 area %), quantitative value: 85% (two process)).

1. temperatureThe diluted solution was cooled to 50 to 60° C. of internal temperature
2. customafter the crystal was precipitated
3. additionFurthermore, water was poured into the solution
4. stirringthe diluted solution was stirred for 1 hour at 20 to 30° C. of internal temperature
5. filtrationThe precipitated crystal was collected by filtration
6. customthe obtained crystal was dried under reduced pressure for 14 hours or more at about 50° C.