HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl (cyanomethyl)phosphonate → HCID 86634346, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl (cyanomethyl)phosphonate | HCID 75676 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 66824283 | HCID 66824283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86634346 | HCID 86634346 | — |
Reaction Steps
To a solution of 1.0 M of potassium tert-butoxide in tetrahydrofuran (5.1 mL) was added dropwise at 0° C. diethyl cyanomethylphosphonate (0.82 mL, 0.0051 mol). The reaction was warmed to rt and 30 min later cooled to 0° C. again. To the reaction mixture was added a solution of 2,2′-(3-oxocyclobutane-1,1-diyl)diacetonitrile (0.5 g, 0.003 mol) in THF (5 mL). The reaction was allowed to warm up to rt gradually and stirred at rt for 2 h. The reaction was quenched with saturated aq. NH4Cl, then extracted with EtOAc. The combined organic layers were washed with brine, dried over MgSO4 and concentrated to give a brown oily crude product, which was used directly in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08158616B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-80e43e7b9da04ad1b7e838d6e5b1420f |
| Source note | uspto-grants-2012_04 |