HuagongsheHuagongshe Chemistry Print Report · For research reference only
Guanidine Hydrochloride → HCID 178478827, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Guanidine Hydrochloride | HCID 5742 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 18319635 | HCID 18319635 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178478827 | HCID 178478827 | 34.3% |
Reaction Steps
To a mixture of ethyl 2,3-dihydro-9-ethoxycarbonyl-1-benzoxepin-4-carboxylate (0.10 g) and guanidine hydrochloride (0.33 g) in N,N-dimethylformamide (2 ml) was added 28% sodium methoxide in methanol (0.66 ml) at room temperature. After the mixture was stirred at room temperature overnight, it was purified by column chromatography on silica gel using a mixture of chloroform and methanol (30:1 to 4:1). The fractions containing objective compound was collected and evaporated in vacuo. The residue was treated with methanol and 4N hydrogen chloride in 1,4-dioxane, and the solvent was evaporated in vacuo. The residue was triturated with ethanol to give (2,3-dihydro-9-guanidinocarbonyl-1-benzoxepin-4-carbonyl)guanidine dihydrochloride (46 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06346527B1 |
| Source dataset | uspto-grants-2002_02 |
| ORD ID | ord-312653dee409460bb7bf4445006ca242 |
| Source note | uspto-grants-2002_02 |