HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13914154, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 13689609 | HCID 13689609 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 13914154 | HCID 13914154 | 24.2% |
Reaction Steps
1.0 g (0.015 mol) of sodium azide is added to 3.0 g (0.007 mol) of 5-bromo-4-nitro-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole in 50 ml of dimethylsulphoxide, the mixture is stirred at room temperature for 15 hours, poured into 150 ml of water and extracted several times with chloroform and ethyl acetate, the combined organic phases are dried over magnesium sulphate and concentrated in vacuo and the oily crude produc is purified by chromatography (silica gel; mobile phase: chloroform/acetone 9:1). 0.68 g (24% of theory) of 5-azido-4-nitro-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole of melting point 84° C.-88° C. is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04770688 |
| Source dataset | uspto-grants-1988_09 |
| ORD ID | ord-244e117507af4511bb3f1fe8f332184b |
| Source note | uspto-grants-1988_09 |