HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22267251, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 22267285 | HCID 22267285 | — |
| Reactant | Boron tribromide dichloromethane | HCID 22277759 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22267251 | HCID 22267251 | 65.8% |
Reaction Steps
A solution of 2-(7-chloro-6-methoxy-2-oxo-4-phenyl-2H-chromen-3-yl)-N-[4-chloro-2-(trifluoromethyl)phenyl]acetamide (Example 178) (3.20 g) in methylene chloride (10 ml) was combined with a 1 M solution of boron tribromide/methylene chloride (31.6 ml, 13.6 mmol), and stirred at room temperature for 3 days. The reaction solution was poured into an ice water, to which concentrated hydrochloric acid was then added. The precipitate was filtered and washed with isopropanol followed by ether to obtain the title compound as a colorless crystal (2.05 g, 64%). An aliquot was recrystallized from THF-isopropyl ether to measure a melting point. Melting point: 246-247° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06974806B2 |
| Source dataset | uspto-grants-2005_12 |
| ORD ID | ord-5aea697fbe5c444188efe0117a2a47be |
| Source note | uspto-grants-2005_12 |