HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 67161596, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | O-(Diphenylphosphinyl)hydroxylamine | HCID 10955453 | — |
| Reactant | HCID 12796522 | HCID 12796522 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67161596 | HCID 67161596 | 84.9% |
Reaction Steps
A mixture of Example 9A (69.1 mg, 0.303 mmol) and KOtBu (1 M in THF, 0.35 mL, 0.35 mmol) in THF (1.5 mL) was stirred for 60 min, and O-(diphenylphosphoryl)hydroxylamine (81.0 mg, 0.348 mmol) and DMF (1.5 mL) were added and stirred 1 hour. The mixture was diluted with EtOAc, washed with 1 N NaOH and water, dried (Na2SO4), filtered, and concentrated to give the title compound as a white solid (62.6 mg), which was used without purification. 1H NMR (300 MHz, DMSO-d6) δ 8.16 (d, 1H), 7.89-7.82 (m, 2H), 7.75 (d, 1H), 7.64-7.51 (m, 3H), 6.65 (s, 2H); LC/MS (APCI) M/Z 244.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629143B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-2a6293cc9c3f4952be35bd473b96f05e |
| Source note | uspto-grants-2014_01 |