HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Chloride → HCID 11682171, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 11683343 | HCID 11683343 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 11682171 | HCID 11682171 | 61.9% |
Reaction Steps
To a solution of N-(3′,3′-dimethyl-3′,4′-dihydro-2′H-spiro[1,3-dioxane-2,10′-pyrimido[1,2-a]indol]-8′-yl)benzenesulfonamide (0.064 g, 0.14 mmol, 1 eq) in CH2Cl2 (4 mL) was added methanesulfonic acid (2 mL). The reaction was stirred at rt overnight and then poured into brine. It was basified to pH 10, saturated with solid NaCl, and extracted with EtOAc. The combined organics were dried over sodium sulfate and concentrated. The crude residue purified by column chromatography using acetone/hexanes (40/60) as an eluent to give the title compound as a yellow foam (0.032 g, 58% ). NMR (400 Mz, DMSO-d6): consistent. MS: (ES−) m/z 368 [M−H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07256198B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-400067b40e4543acaa2791b439cc2248 |
| Source note | uspto-grants-2007_08 |