Potassium Carbonate → HCID 59234646, compound

To a solution of 3-bromo-2(1H)-pyridinone (commercial source: Alfa Aesar) (5 g, 28.7 mmol) in DMF (130 ml) was added K2CO3 (4.8 g, 34.5 mmol). The reaction mixture was stirred at room temperature for 1 hour, then 1-bromo-4-chlorobutane (3.3 ml, 28.7 mmol) was added and the reaction mixture was stirred for 18 hours at room temperature. DMF was evaporated, water was added to the crude and the organic layers were extracted with DCM. The organic layers were combined, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography on silica gel eluting with a gradient of methanol in DCM (from 0 to 5%) to afford the title compound (4.82 g, 63%).

1. stirringthe reaction mixture was stirred for 18 hours at room temperature
2. customDMF was evaporated
3. additionwater was added to the crude
4. extractionthe organic layers were extracted with DCM
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by column chromatography on silica gel eluting with a gradient of methanol in DCM (from 0 to 5%)

ORD record

ord-2babd14e24dc4ea0986b7e878303b813

Source dataset

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08163927B2