HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanesulfonylchloride, 2-chloro- → HCID 56655832, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Pyridinamine, 3-[4-(4-methylphenoxy)phenyl]- | HCID 66747745 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 56655832 | HCID 56655832 | — |
Reaction Steps
To a suspension of NaH (60%, 1.57 g) in THF (dry) (60 ml) was added 2-chloroethanesulfonyl chloride (1.652 mL) at 0° C. and the mixture was stirred for 10 min at the same temperature. A solution of 3-(4-(4-methylphenoxy)phenyl)pyridin-2-amine (2.17 g) in THF (dry) (40 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. Water, EtOAc and IPE were added and the precipitates were collected, washed with water/EtOAc, and dried in vacuo. The precipitates were crystallized from DMSO (15 mL)/EtOH (200 ml) at 80° C. to room temperature to give the title compound (1.91 g) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08575154B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-2c75763ab0744a67be4c1f28797d8f04 |
| Source note | uspto-grants-2013_11 |