HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 44549020, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzenesulfonyl chloride | HCID 7369 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 67001255 | HCID 67001255 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 44549020 | HCID 44549020 | 42% |
Reaction Steps
To a solution of 2-(3′-methanesulfonyl-biphenyl-3-yl)-1-o-tolyl-piperazine hydrochloride (58 mg) in THF (1 mL) sodium hydride (12.3 mg, 60% in mineral oil) was added. After stirring for 30 min at room temperature, benzenesulfonyl chloride was added at 0° C. and stirring was continued at room temperature overnight. Water and ethyl acetate was added, the phases were separated and the inorganic one was extracted with ethyl acetate (×3). The combined organic layers were washed with water, brine, dried (Na2SO4) and concentrated in vacuo. Column chromatography (SiO2, n-heptane/ethyl acetate 2:1,) yielded 4-benzenesulfonyl-2-(3′-methanesulfonyl-biphenyl-3-yl)-1-o-tolyl-piperazine (55 mg, 42%) as colorless oil, MS: 547.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063088B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-f6612eee7ba14ef9847a9b1d6c454c76 |
| Source note | uspto-grants-2011_11 |