HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 1,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 1,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine | HCID 20634959 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate | HCID 20634960 | 90.7% |
Reaction Steps
To a solution of 1,4-bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (83.0 mg, 0.170 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.37 mL, 0.37 mmol), and the mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from ethanol-diethyl ether-hexane to yield the title compound as colorless needles [melting point: 188.0° C. (decomposed)](101.0 mg, yield: 86%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06706703B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-c371c5b1a1fe4433a20455a57571acb6 |
| Source note | uspto-grants-2004_03 |