HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid methylene chloride → 1-(2-Phenyl-1-piperazinyl)ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | (+/-)-1-BOC-4-acetyl-3-phenyl-piperazine | HCID 67083964 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-(2-Phenyl-1-piperazinyl)ethanone | HCID 23198760 | 119.4% |
Reaction Steps
To a solution of 4-acetyl-3-phenyl-piperazine-1-carboxylic acid tert-butyl ester (250 mg, 0.82 mmol) in THF (3 mL) at 0° C. was added 50% TFA/dichloromethane (1 mL). After stirred for 2 h, the reaction mixture was concentrated in vacuo. The residue was diluted with dichloromethane and silica-bound carbonate (2 g, 0.77 mmol/g, Silicycle, Inc.) was added. The reaction mixture was stirred overnight, filtered, and concentrated in vacuo. The residue was purified by flash chromatography (10/1 dichloromethane/methanol with 1% triethyl amine) to provide 1-(2-phenyl-piperazin-1-yl)-ethanone (200 mg, 119%). (M+H)+=205 m/e.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09353096B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-8da7e0cb58cd4eedbe282aa7ffabb9b7 |
| Source note | uspto-grants-2016_05 |