HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 18333003, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 18332937 | HCID 18332937 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18333003 | HCID 18333003 | — |
Reaction Steps
Methanesulfonyl chloride (0.65 ml) was added dropwise to an acetonitrile (20 ml) solution of 3-(pyrrolidin-1-yl)methyl-1, 2,3, 4-tetrahydroquinoline (Reference Example 47; 1.5 g) and triethylamine (2.9 ml) under ice-cooling. The reaction mixture was stirred at the same temperature for one hour, to which was added water and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with a saturated aqueous sodium chloride solution, then dried and concentrated. The residue was purified by alumina column chromatography (eluent: hexane to hexane/ethylacetate=7/1). The crystals were washed with IPE to obtain the entitled compound (1.20 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329389B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-b6d2efac4c23412e90b89549ce1ae161 |
| Source note | uspto-grants-2001_12 |