HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21887532, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 21887245 | HCID 21887245 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21887532 | HCID 21887532 | — |
Reaction Steps
Methylsulfonyl chloride (804 μl) was added to a solution of 5-chloro-1-(2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)-1-pentanone (2.4 g) obtained in Reference Example 121 and triethylamine (1.67 ml) in tetrahydrofuran (30 ml). After stirring at room temperature for 60 minutes, water (50 g) was added, extracted with ethyl acetate, and washed with brine. The organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure to give a pale yellow solid (2.2 g). Further recrystallization from ethanol-diethyl ether afforded the title compound as colorless crystals (1.92 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07462628B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-0d01073f3d1344c189464b2e48c827ae |
| Source note | uspto-grants-2008_12 |