HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 20634976, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 20634975 | HCID 20634975 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 20634976 | HCID 20634976 | 83.4% |
Reaction Steps
To a solution of 1,4-bis[5-(4-chloro-3,5-dimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine (130.0 mg, 0.210 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.45 mL, 0.45 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. The residue was recrystallized from methanol-chloroform-diethyl ether to yield the title compound as a colorless crystalline powder (melting point: 279.0-282.0° C.) (138.0 mg, yield: 83%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06706703B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-be1bce7fdde24f2298ac6c89e0056d2a |
| Source note | uspto-grants-2004_03 |