HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 2-Amino-7-[beta-(p-chloro-phenyl)-ethyl]-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-amino-7-(p-chlorophenylacetyl)-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine | HCID 20436461 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-Amino-7-[beta-(p-chloro-phenyl)-ethyl]-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine dihydrochloride | HCID 20436399 | — |
Reaction Steps
3 gm (9.5 mmols) of 2-amino-7-(p-chlorophenyl-acetyl)-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine were added in portions to a stirred suspension of 3.8 gm (0.1 mol) of lithium aluminum hydride in 150 ml of absolute tetrahydrofuran, and the mixture was stirred overnight. Thereafter, the excess lithium aluminum hydride was decomposed with 2 N sodium hydroxide, the precipitated sodium aluminate was suction-filtered off, and the filtrate was evaporated. The residue was column-chromatographically purified on silicagel with ethyl acetate/methanol (2:1) as the mobile phase, and the dihydrochloride was precipitated with ethanolic hydrochloric acid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04409220 |
| Source dataset | uspto-grants-1983_10 |
| ORD ID | ord-be8833c4171745a983341d2121e3de89 |
| Source note | uspto-grants-1983_10 |