Acetic Acid → 7-Bromothieno(3,2-d)pyrimidin-4-ol

Temperature

120 °C

Thieno[3,2-d]pyrimidin-4(3H)-one (38.0 g, 0.25 mol) was dissolved in acetic acid (143 mL, 2.5 mol), and bromine (40.4 mL, 0.78 mol) diluted with acetic acid (122 mL, 2.1 mol) was slowly added to the solution prepared. The reaction solution was stirred in a sealed reactor for 18 hours at 120° C. The reaction solution was cooled to room temperature and acetic acid was removed by distillation under reduced pressure. The reaction mixture was poured into an ice water to generate a solid compound, and the resulting solid compound was filtered and dried. The title compound was obtained without purification (37.5 g, 65%).

1. additionwas slowly added to the solution
2. customprepared
3. temperatureThe reaction solution was cooled to room temperature
4. customacetic acid was removed by distillation under reduced pressure
5. additionThe reaction mixture was poured into an ice water
6. filtrationthe resulting solid compound was filtered
7. customdried

ORD record

ord-13acca3dcf89470aa420dc50fd1885d8

Source dataset

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09156852B2