HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178502725, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N,O-Dimethylhydroxylamine | HCID 14232 | — |
| Reactant | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178502725 | HCID 178502725 | — |
Reaction Steps
A reaction mixture of 13C (1 g, 3.09 mmol) in DMF (5 mL) was treated with N,O-dimethylhydroxylamine.HCl (0.452 g, 4.64 mmol), BOP (1.778 g, 4.02 mmol) and triethylamine (1.293 mL, 9.28 mmol). The reaction mixture was stirred at room temperature overnight. The mixture was diluted with water and the resulting white solid was collected by filtration, and rinsed with water and air dried to provide 13D (1.2 g, >quantitative yield) as a white solid. 1H NMR (400 MHz, CDCl3) δ ppm 7.29 (d, 4H, J=7.0 Hz); 7.17-7.26 (m, 4H); 7.10-7.16 (m, 2H); 3.61 (s, 3H); 3.56 (s, 4H); 3.08 (s, 3H); 2.44-2.59 (m, 2H); 1.85-1.95 (m, 2H); 1.70-1.82 (m, 2H); 1.28-1.45 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08791257B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-b8dfcfb168654f28a81d4888ccb0a346 |
| Source note | uspto-grants-2014_07 |