Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | Allyltributylstannane | HCID 90628 | — |
| Reactant | HCID 69671577 | HCID 69671577 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 69671657 | HCID 69671657 | — |
Reaction Steps
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), to a solution of 2-bromo-2,2-difluoro-1-(pyrrolidin-1-yl)ethanone (600 mg, 2.63 mmol) in dry toluene (18 mL) was added allyltributyltin (0.84 mL, 2.63 mmol) and AIBN (9 mg, 0.05 mmol) at rt. The reaction mixture was stirred at 100° C. for 1 h. AIBN (9 mg, 0.05 mmol) was then added again and the reaction mixture further stirred at 100° C. for 30 h. The solvent was removed under reduced pressure and the crude residue purified by FC (SiO2 containing 10% KF, hept-EA, 1:0→4:1) to give the title compound as a colorless oil. LC-MS-conditions 08: tR=0.73 min; [M+H]+=190.30.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09187435B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-ee55767f1e8b40009c02be216e1aa863 |
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| Source note | uspto-grants-2015_11 |
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