HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → 5H-Dibenz(b,f)azepine, 10,11-dihydro-2-((4-methyl-1-piperazinyl)methyl)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Iminodibenyl | HCID 10308 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | 5H-Dibenz(b,f)azepine, 10,11-dihydro-2-((4-methyl-1-piperazinyl)methyl)- | HCID 3048897 | 91% |
Reaction Steps
10,11-Dihydro-5H-dibenz [b,f]azepine (250 g) was suspended in a mixture of 600 ml of dichloroethane and 600 ml of acetic acid, and 155 ml of 1-methylpiperazine was added dropwise to the suspension. To the mixture was added 42 g of paraformaldehyde at 50° C. followed by stirring for 6 hours. The solvent was distilled off under reduced pressure and the residue was diluted with ethyl acetate. The solution was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give the product (91%). The obtained product was subjected to the subsequent reaction without particular purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05378701 |
| Source dataset | uspto-grants-1995_01 |
| ORD ID | ord-cf011155c84141b59138b5163e9ca8dd |
| Source note | uspto-grants-1995_01 |