HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 15541117, compound → HCID 14116663, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 15541117 | HCID 15541117 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 14116663 | HCID 14116663 | 77.9% |
Reaction Steps
A suspension of 4-(4′-bromo-biphenyl-4-yl)-4-oxo-butyric acid, methyl ester (2.636 g, 0.00759 mol) in 6 M HCl was refluxed for 214 hours and cooled to room temperature. The solids were filtered and washed with 1 M HCl. The filter cake was partitioned between ethyl acetate and 1 M sodium hydroxide. The aqueous layer was washed twice with ethyl acetate and filtered to remove particulates. The filtrate was rotary evaporated to remove residual ethyl acetate. The solution was stirred and acidified to pH 2 with concentrated HCl solution. The resulting precipitate was filtered, washed with water, and dried with house vacuum (air bleed) give 1.97 g of 4-(4′-bromo-biphenyl-4-yl)-4-oxo-butyric acid as a white solid; mp 198-200° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06307089B2 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-2ad9bc6407804a40962ccc784eb89739 |
| Source note | uspto-grants-2001_10 |