HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanesulfonylchloride, 2-chloro- → HCID 66748620, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 66748381 | HCID 66748381 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66748620 | HCID 66748620 | — |
Reaction Steps
To a suspension of NaH (60%, 29.2 mg) in THF (dry) (2 mL) was added 2-chloroethanesulfonyl chloride (0.046 mL) at 0° C. and the mixture was stirred for 5 min at the same temperature. A solution of 3-(4-phenylcyclohexyl)pyridin-2-amine (36.8 mg) in THF (dry) (2 mL) was added at 0° C. and the mixture was stirred at room temperature under nitrogen overnight. The mixture was quenched with water at 0° C. carefully and extracted with EtOAc. The organic layer was separated, washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography (silica gel, eluted with EtOAc in hexane) and crystallized from EtOAc-hexane to give the title compound (15.7 mg) as an off-white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916551B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-75f3db5efb1443308e017e9b33ed78c1 |
| Source note | uspto-grants-2014_12 |