HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethyl Phosphate → HCID 58415248, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethyl Phosphate | HCID 6535 | — |
| Reactant | HCID 178469011 | HCID 178469011 | — |
| Product | HCID 58415248 | HCID 58415248 | — |
Reaction Steps
A mixture of (E)-ethyl 4-(5-bromo-2-nitrobenzylideneamino)-3-fluorobenzoate (432 mg, 1.09 mmol) and triethyl phosphate (1.5 mL, 9.0 mmol) was irradiated in a microwave instrument at 150° C. for 1.5 h. The cooled reaction mixture was purified by silica gel column chromatography (hexane/ethyl acetate) to give ethyl 4-(5-bromo-2H-indazol-2-yl)-3-fluorobenzoate as pale yellow solid. 1H NMR (400 MHz, CDCl3) δ 8.56 (d, J=2.0 Hz, 1H), 8.25 (t, J=7.8 Hz, 1H), 8.02-7.90 (m, 2H), 7.89 (d, J=0.8 Hz, 1H), 7.66 (d, J=9.2 Hz, 1H), 7.40 (dd, J=1.6, 9.2 Hz, 1H), 4.43 (q, J=7.2 Hz, 2H), 1.44 (t, J=7.2 Hz, 3H); 19F NMR (376 MHz, CDCl3) δ −123.4. MS (ESI) m/z: Calculated: 363.18; Observed: 363.2 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07919519B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-bc1fcd6161be4843aa5214230caf4f83 |
| Source note | uspto-grants-2011_04 |