HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyacetonitrile → HCID 10647295, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyacetonitrile | HCID 7857 | — |
| Reactant | HCID 10716676 | HCID 10716676 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10647295 | HCID 10647295 | — |
Reaction Steps
To a solution of 5-methylamino-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.6 g) in methanol (10 ml) is added glycolonitrile (50%, 0.19 ml) and the mixture is stirred at room temperature for 20 minutes, and then refluxed for 30 minutes. Thereto is added additional glycolonitrile (0.5 ml) and the mixture is refluxed for 5.5 hours. The reaction solution is concentrated and to the resulting residue is added ethyl acetate. The precipitated crystal is collected by filtration, and recrystallized from acetonitrile to give 5-(N-methyl-N-cyanomethylamino)-1-[4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.32 g) as colorless needles, m.p. 227-228° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05985869 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-81db645a579c40fa8b204cad629a813b |
| Source note | uspto-grants-1999_11 |