HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethoxalyl chloride → HCID 59608116, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethoxalyl chloride | HCID 20884 | — |
| Reactant | HCID 67505770 | HCID 67505770 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59608116 | HCID 59608116 | 82.1% |
Reaction Steps
To a solution of (4S)-ethyl 4-amino-5-(3′-chlorobiphenyl-4-yl)-2-methylpentanoate hydrochloride salt (600 mg, 1.74 mmol) in DMF (13.1 mL) is added TEA (0.25 mL, 1.82 mmol) and ethyl 2-chloro-2-oxoacetate (0.19 mL, 1.74 mmol) at room temperature. After stirring this reaction for 1 hour at room temperature, the reaction is quenched with H2O, and diluted in 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 (eluent: heptane/EtOAc=70:30 to 50:50) to give (4S)-ethyl 5-(3′-chlorobiphenyl-4-yl)-4-(2-ethoxy-2-oxoacetamido)-2-methylpentanoate (637 mg). HPLC retention time=1.66 minutes (condition A); MS 446.5 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006249B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-18a0660bc92c4344a33df81bb40f0c50 |
| Source note | uspto-grants-2015_04 |