HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-(2-Bromo-5-fluoro-phenyl)-2-methyl-2H-tetrazole → 4-Fluoro-2-(2-methyl-2H-tetrazol-5-yl)-benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-(2-Bromo-5-fluoro-phenyl)-2-methyl-2H-tetrazole | HCID 21069928 | — |
| Reactant | HCID 178418546 | HCID 178418546 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-Fluoro-2-(2-methyl-2H-tetrazol-5-yl)-benzonitrile | HCID 21069887 | 73.8% |
Reaction Steps
A mixture of intermediate 57, 5-(2-bromo-5-fluoro-phenyl)-2-methyl-2H-tetrazole (650 mg, 2.53 mmol) and CuCN (224 mg, 2.5 mmol) in dimethylformamide (4 mL) was placed in a sealed tube and heated at 100–110° C. for 20 hrs. After cooling, the insoluble material was filtered, and the filtrate concentrated in vacuo. The residue was dissolved in CH2Cl2, washed with aq. 4N HCl and dil. NH4OH, then dried (MgSO4), filtered, and concentrated. The residual solid was purified by column chromatography (SiO2, CH2Cl2) to obtain 375 mg (Yield 73%) of the title compound as an off-white solid; 1H NMR (500 MHz, CDCl3) δ ppm: 4.48 (3H, s) 7.29 (1H, dd, J=7.6, 2.8 Hz) 7.85 (1H, dd, J=8.6, 5.2 Hz) 8.00 (1H, dd, J=9.0, 2.6 Hz); LC/MS m/z 204.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176196B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-0278533f6e7b4735bf3b8bd7028337c7 |
| Source note | uspto-grants-2007_02 |