HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → HCID 57925823, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | Diethyl methylphosphonite | HCID 85063 | — |
| Reactant | Tris(trimethylsilyl)silane | HCID 123134 | — |
| Reactant | 6-Bromonicotinic acid | HCID 238932 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57925823 | HCID 57925823 | — |
Reaction Steps
6-Bromonicotinic acid (150 mg, 0.74 mmol) and diethyl methylphosphonite (1.21 g, 8.91 mmol) were dissolved in toluene and the solution was purged with argon for several minutes. The mixture was brought to reflux and a solution of AIBN (40 mg, 0.22 mmol) and tris trimethylsilylsilane (220 mg, 0.89 mmol) in toluene was added dropwise over 4 hours via syringe pump. The initiator was added via syringe pump over 4 hours. The resulting mixture was reluxed for 16 hours then it was concentrated in vacuo and purified directly by MPLC (0-50% EtOAc:Hex). MS: cal'd 230 (MH+), exp 230 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981874B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-8c82be76d3c0478fb8138dd56601e6dd |
| Source note | uspto-grants-2011_07 |