HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 58997665, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 58997648 | HCID 58997648 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58997665 | HCID 58997665 | — |
Reaction Steps
Pd(OH)2 was carefully wetted down under N2 with 5 mL of MeOH then the product of Step f (0.95 g) dissolved in 5 mL of MeOH was added followed by 5 mL of HOAc. The mixture was hydrogenated overnight on a Parr shaker at 50 psi. Worked up by filtering off the catalyst under N2 through a fiberglass filter paper and vacuum. The filtrate was stripped to obtain white glass. To white glass was added Et2O/saturated NaHCO3 (25 mL) The layers were separated. The aqueous was basified further with 1N NaOH to pH=12 and extracted 3 times with Et2O. The Et2O extracts from the 1N NaOH layer were combined, dried (Na2SO4) and stripped to give 0.40 g of and amber oil as product. MS (ESI) detects (M+H)+=269.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07291744B2 |
| Source dataset | uspto-grants-2007_11 |
| ORD ID | ord-1411dd38f67542fb9b8f9194f23935e8 |
| Source note | uspto-grants-2007_11 |