HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → 4-chloro-7-methylfuro-[3,4-b]-pyridin-5-(7H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Ethyl 4-chloro-2-(1-bromoethyl)nicotinate | HCID 19902854 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-chloro-7-methylfuro-[3,4-b]-pyridin-5-(7H)-one | HCID 19902852 | — |
Reaction Steps
A mixture of ethyl 4-chloro-2-(1-bromoethyl)nicotinate (7.45 g) and sodium bicarbonate (4.00 g) in 50 ml of DMSO is heated at 120°, under nitrogen, for 2 hours, after which it is cooled, diluted with water, filtered and extracted with ether. The combined organic layers are washed with water and concentrated. The residue is taken into ethyl acetate, washed with brine, dried, concentrated and purified by flash chromatography to give 4-chloro-7-methylfuro-[3,4-b]-pyridin-5-(7H)-one, which is then reacted with N-bromosuccinimide and 2,2'-azobis(2-methylpropionitrile), as above, to give 7-bromo-4-chloro-7-methylfuro-[3,4-b]-pyridin-5-(7H)-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05098462 |
| Source dataset | uspto-grants-1992_03 |
| ORD ID | ord-577f714f52a74b5ebae5ea0ca3fb61ad |
| Source note | uspto-grants-1992_03 |