HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromotrimethylsilane → HCID 86641268, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromotrimethylsilane | HCID 76113 | — |
| Reactant | 3-(Diethoxyphosphinyl)propyl 2-propenoate | HCID 86641269 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86641268 | HCID 86641268 | 99% |
Reaction Steps
To a solution of diethyl 3-acryloyloxypropylphosphonate (31.12 g; 0.124 moles) in CH2Cl2 (85 g) is added a solution of trimethylsilyl bromide (40 g; 0.261 moles) in CH2Cl2 (9.2 g) dropwise at room temperature. The mixture is refluxed for 4 hours. The solvent is evaporated on a rotary evaporator under reduced pressure to afford di(trimethylsilyl) 3-acryloyloxypropylphosphonate as a clear, colorless liquid (42.4 g; purity 95% by GC). 1H NMR (CDCl3, δ ppm) 0.006 (s, 9H, CH3—Si), 1.4-1.54 (m, 2H, CH2—P), 1.59-1.72 (m, 2H, CH2—CH2—), 3.91 (t, 2H, CH2—O), 5.55 (dd, 1H, CH═), 5.83 (dd, 1H, CH═), 6.12 (dd, 1H, CH═). 31P NMR (CDCl3, δ ppm) 13.55.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08372516B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-8553b5a8a9c54441a796d045aec64ad6 |
| Source note | uspto-grants-2013_02 |