HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Azide → 3-bromo-5-nitrophenyl-1-methyl-1H-tetrazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 3-Bromo-N-methyl-5-nitrobenzamide | HCID 22252686 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-bromo-5-nitrophenyl-1-methyl-1H-tetrazole | HCID 22252690 | 44.1% |
Reaction Steps
To a solution of 3-bromo-N-methyl-5-nitro-benzamide (0.6 g) in DCM (15 ml) at −15° C. was added triflic anhydride (0.6 ml) and the reaction stirred for 30 min. Sodium azide (226 mg) was added and the reaction allowed to warm to room temperature and stirred further overnight. NaHCO3(aq) was added to neutralise the reaction and the mixture extracted into EtOAc. The organic layer was separated, dried and concentrated in vacuum and the residue purified by flash chromatography (9:1 to 2:8 cyclohexane:EtOAc) to give the title compound (290 mg). Rf=0.51 (3:2 cyclohexane:EtOAc).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE045323E1 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-4d35fc24975a46cd8faf905fd7ed430b |
| Source note | uspto-grants-2015_01 |