HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → Homoveratrylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 3,4-Dimethoxybenzeneacetonitrile | HCID 66727 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Homoveratrylamine | HCID 8421 | — |
Reaction Steps
100 kg. of crystalline 3,4-dimethoxy-benzyl cyanide are hydrogenated in 310 1. of a 80 to 96% aqueous ethanol containing 9 to 12% of ammonia in the presence of 24 kg. of Raney-nickel catalyst pre-treated as described in Example 3 at 48°-60° C under a hydrogen overpressure of 8 to 10 atm. The catalyst is filtered off, the filtrate is evaporated and the residue is subjected to fractionation in vacuo. Thus 95,5 kg. of highly pure 3,4-dimethoxy-beta-phenyl-ethylamine are obtained, purity: nearly 100%. The mono-demethylated beta-phenyl-ethylamine derivative impurity is present at most in traces in such a small amount, which can not be detected by thin layer chromatography.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04126615 |
| Source dataset | uspto-grants-1978_11 |
| ORD ID | ord-f62ae4c6e8854921aadeb629cf79f646 |
| Source note | uspto-grants-1978_11 |