HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium thiocyanate → MLS002639316
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium thiocyanate | HCID 516872 | — |
| Reactant | HCID 178472877 | HCID 178472877 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | MLS002639316 | HCID 3824588 | — |
Reaction Steps
Pd/C (10%, 1.00 g) is added to a solution of 2-hydroxyimino-3-oxo-butyric acid ethyl ester (62.8 mmol) in HCl (1.25 M in EtOH, 75 mL) and the mixture is stirred at RT under a hydrogen atmosphere (4 bar) for 48 h. After filtration through celite and removal of the solvents crude 2-amino-3-oxo-butyric acid ethyl ester hydrochloride is obtained which is dissolved in a mixture of water (220 mL), EtOH (30 mL) and conc HCl (37%, 2.5 mL). A solution of KSCN (49.9 mmol) in water (25 mL) is added and the mixture is stirred for 2 h at reflux. By cooling in an ice bath the desired product precipitates and is collected by filtration.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063099B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-5fce1e814ffb4033b1fc93025d906e6f |
| Source note | uspto-grants-2011_11 |