HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 18319623, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Reactant | HCID 18319514 | HCID 18319514 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18319623 | HCID 18319623 | — |
Reaction Steps
To a mixture of ethyl 9-amino-2,3-dihydro-1-benzoxepin-4-carboxylate (1.0 g) and triethylamine (4.18 ml) in tetrahydrofuran (10 ml) was added dimethylsulfamoyl chloride (2.30 ml) at 5° C. The reaction mixture was stirred overnight at ambient temperature and partitioned between ethyl acetate and 1N hydrochloric acid. The organic layer was washed successively with saturated aqueous sodium bicarbonate and brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel using a mixture of n-hexane and ethyl acetate (4:1) to give ethyl 2,3-dihydro-9-dimethylsulfamoylamino-1-benzoxepin-4-carboxylate (0.89 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06346527B1 |
| Source dataset | uspto-grants-2002_02 |
| ORD ID | ord-4c93ed445ce1419f867f7a0a5687bed4 |
| Source note | uspto-grants-2002_02 |