HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 118046062, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 118045740 | HCID 118045740 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 118046062 | HCID 118046062 | 58.1% |
Reaction Steps
To tert-butyl 4-(3-amino-6-(3-oxocyclopent-1-en-1-yl)pyrazin-2-yl)-2-fluorobenzoate (650 mg, 1.760 mmol) in MeOH (15 ml) was added 15 ml of DCM under stirring until a clear solution was obtained. The solution was purged by nitrogen for 5 min, then Pd/C (300 mg, 10%, Degussa type) was added, and the resultant mixture was degassed by N2 stream for 15 min. After equipped with hydrogen gas balloon, the reaction mixture was stirred at room temperature for 16 h. The reaction mixture was filtered, and the filtrated solution was concentrated, and the crude material was purified by ISCO. (24 g silica gel, 20 to 80% EtOAc in heptane) to afford 380 mg of the desired product as a light yellow solid. 58.1% yield. LC-MS (m/z): (MH+) 372.1, 0.829 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242996B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-62a276afb1554b8fa262cf2c7e620b3d |
| Source note | uspto-grants-2016_01 |