HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 59022520, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 54681977 | HCID 54681977 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59022520 | HCID 59022520 | — |
Reaction Steps
To a stirred solution of Example 36 (0.388 g, 0.763 mmol) in 1,4-dioxane (5 mL) was added 33 wt % HBr in AcOH (1 mL) at room temperature. After 24 h, the resulting white slurry was diluted with Et2O (50 mL), filtered and dried to afford desired product as 1:1:1 product:HBr:dioxane adduct 0.3521 g, 85%). 1H NMR (500 MHz, DMSO-d6) δ: 12.30 (1H, s), 9.48 (1H, t, J=6.4 Hz), 9.17 (1H, s), 7.39-7.36 (2H, m), 7.20-7.15 (2H, m), 4.57-4.48 (2H, m), 4.08-4.04 (2H, m), 3.94-3.84 (2H, m), 3.75-3.69 (1H, m), 3.60-3.49 (6H, m), 3.47-3.31 (4H, m), 2.69-2.62 (1H, m), 2.44-2.38 (1H, m). HRMS (M+H) calcd for C18H20N4O4F: 375.1469; found: 375.1466.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897593B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-99299b64ef5549ce92c1cf0f7bd7d491 |
| Source note | uspto-grants-2011_03 |