HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178426651, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 4-Bromo-3,5-dimethyl-benzonitrile | HCID 11085070 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178426651 | HCID 178426651 | — |
Reaction Steps
A mixture of 4-bromo-3,5-dimethyl-benzonitrile (1.50 g), hydroxylamine hydrochloride (0.90 g), triethylamine (1.8 mL) and ethanol (30 mL) is stirred at reflux temperature for 4 h. After cooling to room temperature, the mixture is concentrated, the residue is taken up in water, and the resulting mixture is extracted with ethyl acetate. The combined extract is washed with brine, dried (Na2SO4), and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 7:3→3:7) to give the title compound. LC (method 11): tR=0.73 min; Mass spectrum (ESI+): m/z=243/245 (Br) [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08642585B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-fe2b26db05e3496a8c9f94e8def1af03 |
| Source note | uspto-grants-2014_02 |