HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formic Acid → HCID 66768992, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | HCID 57708764 | HCID 57708764 | — |
| Catalyst | HCID 178418390 | HCID 178418390 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 66768992 | HCID 66768992 | 78% |
Reaction Steps
A mixture of ethyl 4-[(3-cyanophenyl)oxy]butanoate obtained in Reference Example 41 (8.50 g, 36.4 mmol), 10% palladium carbon (containing 50% water)(12.8 g), formic acid (98 mL) and methanol (80 mL) was stirred at room temperature for 5 hr under hydrogen atmosphere (1 atm). The precipitate was filtered off, and the filtrate was concentrated under reduced pressure. 4N Hydrogen chloride/ethyl acetate solution (15.0 mL, 60.0 mmol) was added to the obtained residue, and the mixture was stirred, and concentrated under reduced pressure. The residue was crystallized from toluene, and the crude crystals were recrystallized from diethyl ether to give the title compound as a white powder (7.79 g, 78%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07915267B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-115d24289ba749348642416f535e2444 |
| Source note | uspto-grants-2011_03 |