HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 1,4-Bis[5-(3,5-dimethoxy-4-methylthiophenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 20634954 | HCID 20634954 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1,4-Bis[5-(3,5-dimethoxy-4-methylthiophenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate | HCID 86587275 | 61% |
Reaction Steps
To a solution of 1,4-bis[5-(3,5-dimethoxy-4-methylthiophenyl)-2-pyridyl]hexahydro-1,4-diazepine (72.0 mg, 0.120 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.24 mL, 0.24 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. Methanol-diethyl ether was added to the residue, and the resulting precipitate was collected to yield the title compound as a pale yellow crystalline powder (melting point: 212.0-217.0° C. (58.0 mg, yield: 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06706703B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-7221d30bc4c34e7d92a219e7bc9efa64 |
| Source note | uspto-grants-2004_03 |