HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetone → HCID 59228757, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetone | HCID 6571 | — |
| Reactant | 2-Pyridinamine, 5-iodo- | HCID 88579 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59228757 | HCID 59228757 | 37.5% |
Reaction Steps
2-Amino-5-iodopyridine (5 g, 22.73 mmol) was dissolved in ethanol (20 mL). Chloroacetone (2.29 mL, 25 mmol) was added and the mixture was heated at reflux overnight. The reaction mixture was evaporated to dryness. The residue was dissolved in DCM (50 mL) and washed with saturated aqueous sodium bicarbonate solution (20 mL). The organic layer was dried over MgSO4, filtered and evaporated. The resulting crude residue (4.8 g) was triturated with ethyl acetate to afford pure title compound (2.2 g). The filtrate was concentrated to dryness, yielding an additional quantity of less pure title compound (2.0 g). δH (CDCl3) 7.33 (m, 4H), 2.48 (s, 3H). LCMS: MH+ 259.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09309243B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-ec32edf4519d4cde9982a4e73f446cd3 |
| Source note | uspto-grants-2016_04 |