HuagongsheHuagongshe Chemistry Print Report · For research reference only
Propargyl bromide → 2,2,7-trifluoro-6-nitro-4-(prop-2-yn-1-yl)-3,4-dihydro-2H-1,4-benzoxazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Propargyl bromide | HCID 7842 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,2,7-trifluoro-6-nitro-2H-benzo[b][1,4]oxazin-3(4H)-one | HCID 66835854 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | 2,2,7-trifluoro-6-nitro-4-(prop-2-yn-1-yl)-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 87173885 | 88.7% |
Reaction Steps
To 2,2,7-trifluoro-6-nitro-2H-benzo[b][1,4]oxazin-3(4H)-one (6.9 g, 27.8 mmol) and potassium carbonate (4.61 g, 33.4 mmol) in dry N,N-dimethylformamide at RT was dropwise added 3-bromoprop-1-yne (80 wt % in toluene; 4.96 g, 33.4 mmol). The resulting mixture was stirred at RT overnight. The reaction mixture was poured in saturated aqueous NH4Cl solution and extracted with ethyl acetate. The combined extracts were washed with aqueous NaCl solution, dried with Na2SO4, concentrated and chased with toluene to yield 7.06 g of the title compound as dark brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08748348B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-d1a3074d518b49589435e8b0b2057f3e |
| Source note | uspto-grants-2014_06 |