HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 178460675, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Phosphine oxide, (chloromethyl)dimethyl- | HCID 74224 | — |
| Reactant | 4-(1-Piperazinylmethyl)benzoic acid | HCID 17606055 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 178460675 | HCID 178460675 | — |
Reaction Steps
To a solution of 4-Piperazin-1-ylmethyl-benzoic acid (4c) and chloro-(dimethyl-phosphinoyl)-methane (5a) in ethanol was added potassium carbonate. The resulting reaction mixture was refluxed, then cooled to room temperature, diluted with brine, acidified to pH-4, and extracted with EtOAc until the aqueous layer showed little or no evidence of product by HPLC. The combined organics were dried over MgSO4 and concentrated on rotary evaporator. The desired product was purified by silica gel flash chromatography.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06706699B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-ede405ec21084346b6e3a0daa2d97f5b |
| Source note | uspto-grants-2004_03 |