HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane → HCID 22051042, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 86591588 | HCID 86591588 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 22051042 | HCID 22051042 | 69.1% |
Reaction Steps
1-tert-butyl-4-{[3-bromo-4-[(2,4-difluorobenzyl)oxy]-6-methyl-2-oxopyridin-1(2H)-yl]methyl}phenylcarbamate (Step 1) (6.14 g, 11.47 mmol) was suspended in 4N HCl in dioxane (5.74 mL, 22.94 mmol). The reaction mixture was stirred at room temperature for 1 hour then diluted with diethyl ether. The precipitate was collected by filtration and washed with diethyl ether (3×30 mL) to afford a tan solid (3.45 g, 69%). 1H NMR (400 MHz, DMF-d6) δ 7.64 (app dt, J=6.58, 8.59 Hz, 1H), 7.31 (ddd, J=2.55, 9.53, 10.61 Hz, 1H), 7.29-7.12 (m, 5H), 6.56 (s, 1H), 5.28 (s, 2H), 5.27 (s, 2H), 2.28 (s, 3H) ES-HRMS m/z 435.0516 (M+H calcd for C20H18BrF2N2O2 requires 435.0514).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07067540B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-565283bb153d4064af8e2afdbf79c7a7 |
| Source note | uspto-grants-2006_06 |