HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 66869298, compound → HCID 88984999, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 66869298 | HCID 66869298 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 88984999 | HCID 88984999 | 76.6% |
Reaction Steps
3-(Benzyloxy)-5-chloro-1-methylpyridin-4(1H)-one (2.70 g, 10.8 mmol) was mixed in 6N HCl (15 mL) and ethanol (10 mL). After being refluxed for 2 hours, the reaction mixture was concentrated by rotary evaporator. The residue was mixed with water (5 mL) and basified to pH 8-9 with concentrated ammonia. An off-white precipitate came out, and the mixture was again concentrated in vacuo to remove volatiles. The off-white solid was collected by suction filtration and dried to give 3-chloro-5-hydroxy-1-methylpyridin-4(1H)-one (1.32 g). Yield=76.6%; 1H NMR (DMSO-D6, 90 MHz) δ(ppm): 7.98 (s, 1H), 7.47 (s, 1H) and 3.67 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073865B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-546899a964304dbfa17c3f0c4e5bebd0 |
| Source note | uspto-grants-2015_07 |