Hydrochloric Acid → 6-Chloro-4-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazin-2(1H)-one

To a tetrahydrofuran solution (200 mL) of 2,4-dichloro-6-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazine (21.0 g, 63 mmol) synthesized in Reference Synthesis Example 1, 1 M sodium hydroxide aqueous solution (128 mL, 128 mmol) was added at room temperature and the resultant solution was stirred for 1 day. To the reaction solution, 1 M sodium hydroxide aqueous solution (32 mL, 32 mmol) was added and the resultant mixture was stirred for 6 hours. To the reaction solution, 1 M sodium hydroxide aqueous solution (19 mL, 19 mmol) was further added and the resultant solution was stirred for 2 hours. After completion of the reaction, pH of the reaction solution was adjusted to 4 by adding 1 M hydrochloric acid. After removing impurities, the resultant mixture was concentrated under reduced pressure to obtain a solid. The solid was collected by filtration, washed with water, and dried under reduced pressure to obtain the title compound (15.2 g, yield 79%).

1. additionwas added at room temperature
2. customAfter completion of the reaction, pH of the reaction solution
3. customAfter removing impurities
4. concentrationthe resultant mixture was concentrated under reduced pressure
5. customto obtain a solid
6. filtrationThe solid was collected by filtration
7. washwashed with water
8. customdried under reduced pressure

ORD record

ord-8f9a4da718f547f5a7ed4891dcdd570d

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09403798B2