HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 20319970, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 20319967 | HCID 20319967 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 20319970 | HCID 20319970 | 82.3% |
Reaction Steps
A solution of 247 mg of fumaric acid in 10 ml of methanol was added to a solution of 750 mg of N-methyl-2,3,4,5-tetrahydro-[1H]-1-benzazepine-3-amine in 30 ml of ethyl acetate and the mixture was concentrated under reduced pressure to 10 ml and was vacuum filtered to obtain 900 mg of raw product. The latter was dissolved in methanol and the solution was filtered. The filtrate was added to isopropanol and the mixture was concentrated until crystallization occured. The mixture was vacuum filtered to obtain 820 mg of di-[N-methyl-2,3,4,5-tetrahydro-[1H]-1-benzazepine-3-amine] fumarate in the form of colorless crystals melting at 190° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04100278 |
| Source dataset | uspto-grants-1978_07 |
| ORD ID | ord-5c5dcecb76a841658838e1866e6ab2d9 |
| Source note | uspto-grants-1978_07 |