HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 12096250, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 12096239 | HCID 12096239 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12096250 | HCID 12096250 | 57.2% |
Reaction Steps
To sodium hydride (40 mg, 1.0 mmol) in tetrahydrofuran (10 mL) at 0° C. was added 7-bromo-N,N-diethyl-1,2-benzisothiazole-2(3H)-ethanamine 1,1-dioxide (0.26 g, 1.0 mmol). The reaction was stirred for 20 min and treated with methyl iodide (0.06 mL, 1.3 mmol). The resulting mixture was stirred at ambient temperature over 18 h, poured into ice water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate and concentrated in vacuo. The crude material was purified by a flush chromatography ((ethyl acetate/hexane, 1:4) to afford 7-bromo-2,3-dihydro-2-methyl-1,2-benzisothiazole 1,1-dioxide (0.15 g, 56%). LRMS (ES−): 262.0 (M−H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06689770B2 |
| Source dataset | uspto-grants-2004_02 |
| ORD ID | ord-62ec48e422ac462e9c0ddabb86ba1f2b |
| Source note | uspto-grants-2004_02 |