HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 17751567, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Aminomethyl-1,4-benzodioxane | HCID 15053 | — |
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 17751567 | HCID 17751567 | — |
Reaction Steps
Racemic 2,3-dihydro-1,4-benzdioxin-2-ylmethylamine (8.25 g, 5.0 mmol) and triethylamine (1.52 g, 15 mmol) were combined in DMF (10 mL) and cooled in an ice bath as dimethylsulfamoyl chloride (1.44 g, 10 mmol) was added. The reaction mixture was then stirred for 3 hr with continued cooling. The reaction mixture was partitioned between ethyl acetate and water, and the ethyl acetate solution was washed with brine, dried (MgSO4) and evaporated in vacuo to yield an oil. The oil was purified using flash column chromatography (ethyl acetate:Heptane—1:1) to yield a white solid, which was recrystallized (ethyl acetate/Hexane) to yield the title compound as a white floccular solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08716231B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-396a1eaaaa354f85b04738bf1225adee |
| Source note | uspto-grants-2014_05 |