HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 69732326, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | HCID 22482074 | HCID 22482074 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69732326 | HCID 69732326 | — |
Reaction Steps
A mixture of (3-chloro-benzyl)-(6-chloro-pyrazin-2-yl)-amine (I-2a) (71.0 mg, 0.28 mmol), piperazine-1-carboxylic acid tert-butyl ester (260.2 mg, 1.40 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (208.9 μL, 1.40 mmol) in 1.0 mL of ethanol was refluxed for 18 h under nitrogen. The reaction was then cooled to ambient temperature and poured into 20 mL of water. This was extracted 2×30 mL of ethyl acetate and the combined organic extracts were washed with 3×15 mL water followed by 15 mL of brine. The organic layer was then dried over sodium sulfate, filtered and concentrated in vacuo to a yellow residue that was chromatographed (prep. TLC, 1:1 hexane:ethyl acetate) to give the title compound (I-2b) as a white solid, 13.5 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06894050B2 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-49a5cee1df4c448395b88e88c61dbb02 |
| Source note | uspto-grants-2005_05 |