HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 5-Methylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 2,3,4,5-Tetrahydro-1-benzoxepin-5-amine | HCID 15619698 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-Methylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine | HCID 22391790 | 74.7% |
Reaction Steps
1.54 g (13.4 mmol) of methanesulfonyl chloride were added dropwise with ice cooling to a solution of 2.0 g (12.2 mmol) of 5-amino-2,3,4,5-tetrahydro-1-benzoxepine (Example 6b) and 3.7 g (36.6 mmol) of triethylamine in 40 ml of THF. The mixture was allowed to come to RT and was stirred overnight and treated with 50 ml of water, and the THF was distilled off in vacuo. The residue was diluted with a further 50 ml of water and stirred for 3 h, and the deposited product was filtered off with suction. After drying in vacuo, 2.2 g of 5-methylsulfonylamino-2,3,4,5-tetrahydro-1-benzoxepine were obtained, m.p. 105-106° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06333349B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-c3b47cb6ef514ef2a80739637f0a4234 |
| Source note | uspto-grants-2001_12 |