HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → 2-(Methylamino)-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2-Chloro-1-[4-(naphthalene-2-sulfonyl)piperazin-1-yl]ethan-1-one | HCID 2405875 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2-(Methylamino)-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone | HCID 67980994 | 22.9% |
Reaction Steps
To a stirred solution of 2-chloro-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone (compound 5, 0.1 g, 0.85 mmol) in THF (10 mL) diisopropyl ethyl amine (81 mg, 0.62 mmol) was added at 0° C. followed by methyl amine solution (30% solution, 10 mL). The reaction mixture was allowed to stir for overnight at room temperature. The reaction mixture was poured into a large volume of water (50 mL) and the solution was extracted with ethyl acetate. The combined organic extract was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude material was purified by column chromatography to obtain the title compound (20.0 mg, 22.90% yield) as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115086B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-3633194601344ba398ef464875931c0e |
| Source note | uspto-grants-2015_08 |