HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Phenylbenzoyl chloride → HCID 11046468, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Phenylbenzoyl chloride | HCID 84151 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Propanedioic acid, 2-amino-, 1,3-diethyl ester, hydrochloride (1:1) | HCID 3084143 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 11046468 | HCID 11046468 | 95% |
Reaction Steps
4-Phenylbenzoyl chloride (4.3 g) was added little by little to a chloroform (80 mL) solution of diethyl aminopropanedioate hydrochloride (4.3 g) and TEA (8.4 mL) under ice cooling, and the mixture was stirred for 3 hours at the same temperature. A saturated aqueous solution of sodium hydrogen carbonate was added to the reaction mixture, and the mixture was extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, and the desiccant was filtered out. Then, the solvent was distilled off under reduced pressure, and the resulting residue was purified by OH type silica gel column chromatography (chloroform/methanol=20/1) to obtain diethyl [(biphenyl-4-ylcarbonyl)amino]propanedioate (white solid) (6.7 g, 95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073821B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-76cae45ea50b49f491871e5f0216fc9e |
| Source note | uspto-grants-2015_07 |