HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → (2,6-Dichloro-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | (1S)-1,2,3,4-Tetrahydro-N-methyl-1-naphthalenamine | HCID 7128547 | — |
| Reactant | (2,6-Dichloro-3-hydroxymethyl-pyridin-4-yl)-pyrrolidin-1-yl-methanone | HCID 59678084 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | (2,6-Dichloro-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone | HCID 72355817 | — |
Reaction Steps
A mixture of (2,6-dichloro-3-hydroxymethyl-pyridin-4-yl)-pyrrolidin-1-yl-methanone (400 mg, 1.45 mmol) and SOCl2 (1 mL) in CH2Cl2 (10 mL) is stirred at room temperature for 1 hour, and then concentrated. The residue is treated with K2CO3 (1.0 g, 7.2 mmol), CH3CN (10 mL) and (S)-methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amine (250 mg, 1.55 mmol). The resulting mixture is stirred at room temperature overnight. EtOAc (50 mL) and water (40 mL) are added to the residue. The organic layer is separated, washed once with brine, dried (Na2SO4) and concentrated. The residue is chromatographed on silica gel (4:1 hexane:EtOAc) to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07863454B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-0a6ed2600bcd49f9bd544f8ed9589630 |
| Source note | uspto-grants-2011_01 |