HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetamidine monohydrochloride → HCID 136348387, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetamidine monohydrochloride | HCID 67170 | — |
| Reactant | Sodium methanolate methanol | HCID 23694274 | — |
| Reactant | HCID 86721445 | HCID 86721445 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 136348387 | HCID 136348387 | 82.5% |
Reaction Steps
[step 2] (E)-ethyl 2-{[11-(1-cyanoethylidene)-3-fluoro-6,11-dihydrodibenzo[b,e]oxepin-8-yl]methyl}-3-oxohexanoate (1.18 g, 2.71 mmol) obtained in step 1 was dissolved in methanol (14 mL), acetimidamide hydrochloride (640 mg, 6.77 mmol) and 28% sodium methoxide methanol solution (1.83 mL, 9.48 mmol) were added, and the mixture was stirred at room temperature for 2 hr. The mixture was concentrated under reduced pressure, methanol was added to the obtained residue, and the precipitated crystals were collected by suction filtration to give (E)-2-{3-fluoro-8-[(2-methyl-6-oxo-4-propyl-1,6-dihydropyrimidin-5-yl)methyl]dibenzo[b,e]oxepin-11(6H)-ylidene}propanenitrile (960 mg, 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969345B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-0b6f8fc3b4784b5cb5e338ba0a6ad1c0 |
| Source note | uspto-grants-2015_03 |