HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → (3,4-Dimethoxy-bicyclo[4.2.0]octa-1,3,5-trien-7-yl)-methylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 3,4-Dimethoxybicyclo[4.2.0]octa-1,3,5-triene-7-carbonitrile | HCID 290544 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | (3,4-Dimethoxy-bicyclo[4.2.0]octa-1,3,5-trien-7-yl)-methylamine | HCID 423512 | — |
Reaction Steps
Introduce 4,5-dimethoxy-1-cyano-benzocyclobutane (6 kg), methanol (30 liters), Raney nickel (0.6 liters) and ammonia (7.32 kg) into a hydrogenator. After having purged with nitrogen and then with hydrogen, hydrogenate at 60° C. and at 30 bar until the theoretical amount of hydrogen has been absorbed. After returning to 20° C., filter off the catalyst, rinsing it with methanol, and then evaporate off the solvent. The title compound is obtained in the form of an oil, in a quantitative yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06982350B2 |
| Source dataset | uspto-grants-2006_01 |
| ORD ID | ord-81c874d1c78a4007903f142a7348f84d |
| Source note | uspto-grants-2006_01 |