HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 25142339, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 2-Pyrrolidone | HCID 12025 | — |
| Reactant | HCID 57733278 | HCID 57733278 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 25142339 | HCID 25142339 | 56% |
Reaction Steps
To a solution of 2-pyrrolidinone (0.1 ml) in tetrahydrofurane (2 ml) sodium hydride (20 mg, 60% dispersion in mineral oil) was added. The reaction mixture was stirred at ambient temperature until the gas evolution ceased then 3-bromomethyl-1-oxo-2-phenyl-1,2-dihydro-isoquinoline-4-carboxylic acid ((S)-1-phenyl-propyl)-amide (30 mg) was added. After 30 min acetic acid (0.05 ml) was added and volatiles were removed in vacuo. The product was purified by flash chromatography on SiO2 (5 g, 1,2-dichloroethane then gradient 50% to 100% ethyl acetate in heptane) to give 17 mg of white solid. Yield 56%. LC-MS (m/z) 480.5 (MH+); tR=1.21.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08173639B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-9436dbc2075548558a87b2ed7f28f472 |
| Source note | uspto-grants-2012_05 |