HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 66783136, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 5-Fluoro-2-nitrobenzotrifluoride | HCID 223094 | — |
| Reactant | 3-Methyl-2-ketopiperazine | HCID 5106600 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66783136 | HCID 66783136 | 24.5% |
Reaction Conditions
| Temperature | 140 °C |
|---|
Reaction Steps
A mixture of 3-methyl-2-ketopiperazine (200 mg, 1.75 mmol), 5-fluoro-2-nitrobenzo-trifluoride (366 mg, 1.75 mmol), N,N-diisopropylethylamine and N,N-dimethylformamide (1 mL) was heated at 140° C. for 10 min under microwave irradiation, then partitioned between sat. aq. ammonium chloride solution and EtOAc. The organic layer was washed with brine, dried (MgSO4), filtered, and evaporated. Chromatography (SiO2; heptane/EtOAc 4:1) produced the title compound (130 mg, 24%). Yellow solid, MS: 304.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08138175B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-9b70964d591f447797649896ba74d67b |
| Source note | uspto-grants-2012_03 |