HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → 4-Chloro-N-methylpyridine-2-carboxamide--hydrogen chloride (1/1)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | 4-Chloro-N-methylpicolinamide | HCID 1476814 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4-Chloro-N-methylpyridine-2-carboxamide--hydrogen chloride (1/1) | HCID 46781006 | — |
Reaction Steps
420 g of a solution of 4-chloro-N-methylpyridine-2-carboxamide (prepared according to WO2006/034796) in toluene (approx. 30% w/w) and 48.8 g of ethanol were charged into a reaction flask. 67.2 g of acetyl chloride was added with stirring to such a degree that the temperature of the reaction mixture did not exceed 30° C. After stirring further at room temperature for 1.5 h the product was filtered off, washed with toluene (212 g) and dried under reduced pressure (30° C., 80 mbar). In this way 156 g (quantitative yield) of 4-chloro-N-methyl-pyridine-2-carboxamide hydrochloride were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08748622B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-1009b61a810a402e9d578a174dfa6686 |
| Source note | uspto-grants-2014_06 |