HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 117974229, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 117974232 | HCID 117974232 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Product | HCID 117974229 | HCID 117974229 | 51.6% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A mixture of 1.09 g of 3-methyl-6-trifluoromethyl-1,3-dihydro-imidazo[4,5-b]pyridin-2-one, one drop of dimethylformamide and 10 g of phosphorus oxychloride was stirred at 100° C. for 3 hours. The cooled reaction mixture was poured to a saturated aqueous sodium bicarbonate solution, and the mixture was extracted twice with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 0.61 g of 2-chloro-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09120792B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-3aff0ac0f0ba45ef8d77e4f556130336 |
| Source note | uspto-grants-2015_09 |