HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-(4-chlorobenzyl)-3-hydroxypyridin-2(1H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 67155133 | HCID 67155133 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-(4-chlorobenzyl)-3-hydroxypyridin-2(1H)-one | HCID 52912219 | — |
Reaction Steps
To a solution of 3-(tert-butyldimethylsilanyloxy)-1-(3-chlorobenzyl)-1H-pyridin-2-one, 2, (2.36 g, 10 mmol) in EtOAc (25 mL) as added 5 M HCl (25 mL) with vigorous stirring at room temperature. The reaction was monitored by TLC for the disappearance of starting material and was complete within 30 minutes. The organic layer was decanted and the aqueous phase extracted with dichloromethane (2×50 mL). The combined organic layers were dried over Na2SO4 and the solvent removed under reduced pressure. The crude product was recrystallized from dichloromethane. The yield was nearly quantitative. 1H NMR (360 MHz, DMSO-d6) δ ppm 5.12 (2H, s); 6.13 (1H, t, J=7.04); 6.71 (1H, dd, J=7.04, 1.59); 7.23-7.28 (2H, m); 7.36-7.43 (2H, m); 9.10 (1H, br. s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08536181B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-cb5be109acf34a3dbe7b89528e30b867 |
| Source note | uspto-grants-2013_09 |