HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 22485460, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 22485461 | HCID 22485461 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 22485460 | HCID 22485460 | 79.6% |
Reaction Steps
To a solution of 1,4-bis[2-(3,4,5-trimethoxyphenyl)-5-pyridyl]hexahydro-1,4-diazepine (88.0 mg, 0.150 mmol) in methanol-methylene chloride (1:1, 4.0 mL) was added a 1.0 M aqueous methanesulfonic acid solution (0.30 mL, 0.30 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-methylene chloride-diethyl ether to yield the title compound as yellow prisms (melting point: 246.0-248.0° C.)(93.0 mg, yield: 79%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06890940B2 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-6c80fcd10cc441fd8914da67618a58bf |
| Source note | uspto-grants-2005_05 |