HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 2-(4-(S-Methyl-N-(methylsulfonyl)sulfonimidoyl)benzyl)isoindoline-1,3-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 2-(4-(S-Methylsulfonimidoyl)benzyl)isoindoline-1,3-dione | HCID 86711629 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(4-(S-Methyl-N-(methylsulfonyl)sulfonimidoyl)benzyl)isoindoline-1,3-dione | HCID 86711628 | — |
Reaction Steps
A solution of 2-(4-(S-methylsulfonimidoyl)benzyl)isoindoline-1,3-dione (preparation 17b, 2.50 g, 7.95 mmol) and triethylamine (2.2 mL, 16 mmol) in dichloromethane (20 mL) is cooled at 0° C. and treated with methanesulfonyl chloride (620 μL, 8.0 mmol). The mixture is stirred at this temperature for 1.5 h and then washed with water. The organic layer is concentrated under reduced pressure, and the residue is suspended in a mixture of methanol and water. The precipitate is filtered, washed with water, and dried. Yield: 273 mg (8% of theory); ESI mass spectrum: [M+H]+=393, r.t. HPLC: 0.44 min (X012_S01).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09346794B1 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-64095652589442a28667ef95c9615ec7 |
| Source note | uspto-grants-2016_05 |