HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 86635501, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Propargyl bromide | HCID 7842 | — |
| Reactant | Hydrazine, (4-chlorophenyl)-, hydrochloride (1:1) | HCID 71600 | — |
| Catalyst | Tetrabutylammonium Chloride | HCID 70681 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 86635501 | HCID 86635501 | 48% |
Reaction Steps
4-Chlorophenylhydrazine hydrochloride (550 mg, 3 mmol) was added to a vigorously stirred mixture of tetra-n-butylammonium chloride (42 mg, 0.15 mmol) in 50% aqueous sodium hydroxide (3 mL) followed by 80% propargyl bromide in toluene (490 mg, 3.3 mmol). The reaction was stirred at room temperature for 20 h. The reaction was diluted with water (30 mL) and extracted with chloroform (3×10 mL). The combined organic layer was dried (Na2SO4), filtered and concentrated under reduced pressure to a dark brown oil (530 mg). The oil was subjected to column chromatography (silica gel, eluent: 50% dichloromethane in hexanes) to give an orange solid (260 mg, 48%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338447B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-869e98ed0bdf41329503068bc6c20e37 |
| Source note | uspto-grants-2012_12 |