HuagongsheHuagongshe Chemistry Print Report · For research reference only
Heptafluorobutyric acid → HCID 178506194, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Heptafluorobutyric acid | HCID 9777 | — |
| Reactant | 4-Chloro-5-[4-chloro-2-(trifluoromethyl)phenyl]benzene-1,2-diamine | HCID 86699577 | — |
| Product | HCID 178506194 | HCID 178506194 | 68% |
Reaction Steps
A solution of 4-chloro-5-[4-chloro-2-(trifluoromethyl)phenyl]benzene-1,2-diamine (100 mg, 0.31 mmol, 1.00 equiv) in heptafluorobutanoic acid (5 ml) was stirred overnight at 80° C. in an oil bath and then quenched with ice-water (30 ml). The pH value of the solution was adjusted to 8 with saturated aqueous sodium carbonate and extracted with ethyl acetate (50 ml×3). The combined organic layers were dried over anhydrous sodium sulfate and concentrated under vacuum to give a residue, which was purified by Pre-TLC with 10% ethyl acetate in petroleum ether to produce 5-chloro-6-[4-chloro-2-(trifluoromethyl)phenyl]-2-(heptafluoropropyl)-1H-1,3-benzodiazole as a off-white solid (105.8 mg, 68%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09000187B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-b7a822fca7bc4c7a8da9b6cbff492794 |
| Source note | uspto-grants-2015_04 |