HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 21999531, compound → HCID 21999543, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 21999531 | HCID 21999531 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Hydrogen Bromide | HCID 260 | — |
| Product | HCID 21999543 | HCID 21999543 | 87% |
Reaction Steps
A solution of Compound 45 (450 mg, 1.17 mmol) in 5 mL acetic acid and 5 mL 48% hydrobromic acid is heated for 48 hours at reflux. The reaction mixture is worked up as above, and the crude product is purified by column chromatography to yield 362 mg (87%) of Compound 46 as a colorless solid. 19F-NMR (d6 -DMSO) 139.80 (m, 1 F); 141.69 (dd, J=10.0, 20.1 Hz, 1 F); 143.05 (dt, J=5.8, 23.1 Hz, 1 F); 155.48 (dd, J=10.2, 22.8 Hz, 1 F); 155.67 (s, 1 F); 156.27 (dd, J=5.8, 20.5 Hz, 1 F); 158.57 (t, J=22.2 Hz, 1 F); 162.5 (b, 1 F).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06162931 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-12137f89bd3d4b178a849dc8812bb283 |
| Source note | uspto-grants-2000_12 |