HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 44467321, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,4-Dichloro-5-fluoropyrimidine | HCID 250705 | — |
| Reactant | 4-Piperidinemethanol | HCID 420771 | — |
| Reactant | 1-[4-(4-Aminophenyl)piperazin-1-yl]ethan-1-one | HCID 736269 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 44467321 | HCID 44467321 | 22.5% |
Reaction Steps
A mixture of 2,4-dichloro-5-fluoropyrimidine (167 mg, 1.00 mmol), 4-piperidinemethanol (115 mg, 1.00 mmol) and DIEA (0.400 mL, 2.30 mmol) in CH3CN (4 mL) was stirred at room temperature for 2 h. It was concentrated in vacuo. The residue was dissolved in nBuOH (6 mL). 3 mL of the nBuOH solution was taken, to which 1-(4-(4-aminophenyl)piperazin-1-yl)ethanone (120 mg, 0.55 mmol) was added. The solution was stirred at 116° C. for 20 h. nBuOH was removed in vacuo. The residue was purified by HPLC to give the titled compound (53 mg). MS 429.3 (M+H); UV 207.8, 266.8 nm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08258144B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-99f73b306f71497697ff13ffc7363fc9 |
| Source note | uspto-grants-2012_09 |