HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67173340, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 67171796 | HCID 67171796 | — |
| Solvent | Boron tribromide | HCID 25134 | — |
| Product | HCID 67173340 | HCID 67173340 | — |
Reaction Steps
N-(1-Hydroxy-1,3-dihydro-benzo[c][1,2]oxaborol-6-yl)-2-methoxy-4-nitro-benzenesulfonamide (200 mg, 0.55 mmol) was dissolved in 1 M BBr3 in CH2Cl2 (5.0 mL, 5.0 mmol) and the resulting soln was stirred at rt O/N. H2O was the resulting precipitate was isolated by filtration to give the title compound as a white solid: yield; 160 mg (83%). mp 198-199° C.; 1H NMR (400 MHz, DMSO-d6) δ (ppm): 11.98 (s, 1H), 10.22 (s, 1H), 9.18 (s, 1H), 7.89-7.87 (m, 1H), 7.67-7.63 (m, 2H), 7.48 (s, 1H), 7.23-7.18 (m, 2H), 4.84 (s, 2H); MS (ESI) m/z=349 (M−1, negative); HPLC purity: 95.49% (MaxPlot 200-400 nm), 95.48% (220 nm).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461134B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-6af1bd8cac3948dfb74da98e136249c0 |
| Source note | uspto-grants-2013_06 |