HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethoxalyl chloride → HCID 59607653, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethoxalyl chloride | HCID 20884 | — |
| Reactant | (R)-ethyl 3-amino-4-(3'-chlorobiphenyl-4-yl)butanoate hydrochloride | HCID 86648190 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59607653 | HCID 59607653 | 83.8% |
Reaction Steps
To a solution of (R)-ethyl 3-amino-4-(3′-chlorobiphenyl-4-yl)butanoate hydrochloride (500 mg, 1.57 mmol) in DMF (11 mL) is added TEA (0.23 mL, 1.65 mmol) and ethyl 2-chloro-2-oxoacetate (0.18 mL, 1.57 mmol) at room temperature. After stirring for 1 hour at room temperature, the reaction is quenched with H2O, and the crude is diluted with EtOAc. The organic layer is washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The obtained residue is purified by flash column chromatography on silica gel (eluent: heptane/EtOAc=70:30 to 50:50) to give (R)-ethyl 4-(3′-chlorobiphenyl-4-yl)-3-(2-ethoxy-2-oxoacetamido)butanoate (550 mg). HPLC retention time=1.88 minutes (condition A); MS (m+1)=418.3
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08822534B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-48895012827c4b0fa720b735b9e2f50d |
| Source note | uspto-grants-2014_09 |