HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → HCID 18001025, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 18001092 | HCID 18001092 | — |
| Reactant | HCID 70033094 | HCID 70033094 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18001025 | HCID 18001025 | 38.5% |
Reaction Steps
To a mixture of 1-[4-(1-piperazinyl)-2-chlorobenzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.25 g), 37% formaldehyde (0.45 g) and sodium tetrahydro-1H-benzazepine (0.25 g), 37% formaldehyde (0.45 g) and sodium (0.12 g) under ice-cooling, and the mixture is stirred at room temperature for one hour. To the reaction solution is added ethyl acetate, and the mixture is washed with a 2N aqueous sodium hydroxide solution and distilled water. The organic layer is dried over magnesium sulfate, filtered, and concentrated, and the resulting residue is purified by silica gel column chromatography (solvent; dichloromethane:methanol=10:1) to give 1-[4-(4-methyl-1-piperazinyl)-2-chlorobenzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.10 g) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06642223B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-170a33be0fb1413b8a5c1844ac81996f |
| Source note | uspto-grants-2003_11 |