HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allyltributylstannane → 5-Allyl-2,1,3-benzoxadiazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allyltributylstannane | HCID 90628 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | 5-Bromo-2,1,3-benzoxadiazole | HCID 2776298 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 5-Allyl-2,1,3-benzoxadiazole | HCID 59568714 | — |
Reaction Steps
5-Bromo-2,1,3-benzoxadiazole (10 g, 50.3 mmol) was dissolved in toluene (300 mL) and treated with lithium chloride (6.39 g, 151 mmol), Pd(Ph3P)4 (2.90 g, 2.51 mmol), and allyltributylstannane (18.66 ml, 60.3 mmol). Degassed and refluxed the mixture under N2 for 3 hrs. The reaction mixture turned black. Poured the reaction mixture into water and extracted with ethyl acetate. The organic layer was separated, washed with brine, dried, and evaporated to dryness. The residue was chromatographed through 120 g ISCO Redi-Sep column and eluted with 0-10% ethyl acetate/hexane to yield 5-(prop-2-en-1-yl)-2,1,3-benzoxadiazole.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09018211B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-a4a5c502e10b4191b1b903c0d609fe21 |
| Source note | uspto-grants-2015_04 |