HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Diethyl (t-Butyldimethylsiloxy)methylphosphonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Dimethylaminopyridine | HCID 21885 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Reactant | Diethyl phosphonomethanol | HCID 76513 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Diethyl (t-Butyldimethylsiloxy)methylphosphonate | HCID 12606850 | — |
Reaction Steps
To a stirred solution of diethyl hydroxylmethylphosphonate (2.13 g, 12.7 mmol), triethylamine (2.12 ml, 15.2 mmol) and dimethylaminopyridine (77 mg, 0.63 mmol) in dichlormethane at 0° C. under argon, at r.t., was added t-butyldimethylsilyl chloride (1.85 g, 12.8 mmol) in dichloromethane (5 ml). After 14 hr the resulting slurry was poured into water (100 ml) and extracted with dichloromethane (2×100 ml). The organic extracts were dried (Na2SO4), concentrated in vacuo and the resulting oil chromatographed on silica gel eluted with ethylacetate:hexanes (1:1, v:v) to afford the title compound as a clear oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05362906 |
| Source dataset | uspto-grants-1994_11 |
| ORD ID | ord-257fbb3faf53435391ee767d45efb057 |
| Source note | uspto-grants-1994_11 |