HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 67324135, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 67323684 | HCID 67323684 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67324135 | HCID 67324135 | 107.2% |
Reaction Steps
A solution of 1,1-dimethylethyl 4-[(4-cyano-2-methylphenyl)sulfonyl]-1-piperazinecarboxylate (may be prepared as described in Intermediate 8; 3.33 g, 9.11 mmol) and TFA (10 ml, 130 mmol) in dry dichloromethane (10 ml) was stirred at rt for 1 h, then concentrated in vacuo, azeotroping with toluene (25 ml) to give a brown oil. This was partitioned between DCM (50 ml) and sat. aq NaHCO3 (50 ml), then the aqueos layer extracted with DCM:EtOH (3:1, 40 ml). The combined organics were passed through a hydrophobic frit and concentrated in vacuo to give the title compound (2.59 g) as a yellow oil. The product became a pale yellow solid on standing.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697703B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-8576459bb61c41a29394d5a7f404e1b2 |
| Source note | uspto-grants-2014_04 |