HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-(tetrahydro-2H-pyran-4-ylmethyl)-1-(2-thiophenylsulfonyl)piperazine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Thiophenesulfonyl chloride | HCID 85518 | — |
| Reactant | 2-((tetrahydro-2H-pyran-4-yl)methyl)piperazine | HCID 66582363 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(tetrahydro-2H-pyran-4-ylmethyl)-1-(2-thiophenylsulfonyl)piperazine hydrochloride | HCID 70655430 | 76.6% |
Reaction Steps
A 100 mL round-bottomed flask was charged with 2-((tetrahydro-2H-pyran-4-yl)methyl)piperazine (0.950 g, 5.16 mmol), 20 mL of CH2Cl2, triethylamine (0.790 mL, 5.67 mmol), and 2-thiophenesulfonyl chloride (0.942 mL, 5.16 mmol, Sigma-Aldrich, St. Louis, Mo.). After 15 min at room temperature, the mixture was diluted with water (50 mL) and CH2Cl2 (50 mL), the organics were separated, dried (MgSO4) and concentrated to give a dark oil. To this oil was added 50 mL of ether and 10 mL of 1N HCl in ether. The resulting white precipitate was collected by filtration to give 3-(tetrahydro-2H-pyran-4-ylmethyl)-1-(2-thiophenylsulfonyl)piperazine hydrochloride (1.45 g) as an orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08431563B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-97ced884922a4ef9bc9e43342be84845 |
| Source note | uspto-grants-2013_04 |