Bromine → HCID 89655859, compound

To a solution of Example 288c (0.671 g, 3.87 mmol) and sodium acetate (0.318 g, 3.87 mmol) in acetic acid (8.50 mL) was added bromine (0.201 mL, 3.91 mmol) dropwise as a solution in acetic acid (1.7 mL). The reaction mixture was stirred at 40° C. for 3 hours. Bromine (0.05 mL) was added, and the reaction mixture was stirred at 40° C. for 2 hours. The reaction mixture was cooled to ambient temperature and quenched with 100 mL of 10% aqueous sodium thiosulfate. The resulting suspension was filtered, and the solid collected and dried for 16 hours to provide the title compound (0.64 g, 66%).

1. stirringthe reaction mixture was stirred at 40° C. for 2 hours
2. temperatureThe reaction mixture was cooled to ambient temperature
3. customquenched with 100 mL of 10% aqueous sodium thiosulfate
4. filtrationThe resulting suspension was filtered
5. customthe solid collected
6. customdried for 16 hours

ORD record

ord-f14a66215ab945fcb59be10991922590

Source dataset

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09296741B2