HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 20378679, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 20378670 | HCID 20378670 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 20378679 | HCID 20378679 | — |
Reaction Steps
A mixture of 7.1 g. of 2,3,4,4a-tetrahydro-3-methyl- 1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, 3.5 g. of lithium aluminum hydride and 450 ml. of dry tetrahydrofuran is refluxed for 20 hours under a nitrogen atmosphere. The mixture is cooled and 20 ml. of concentrated ammonium hydroxide is carefully added. The mixture is filtered and the filter cake is washed with isopropanol. The filtrate is concentrated to give 5.7 g. of product as a viscous oil. A 3.5 g. portion is dissolved in acetone and treated with a saturated solution of fumaric acid in acetone. Filtration gives 3.3 g. of the product as the fumaric acid salt, m.p. 178°-188°. Recrystallization from isopropanol gives 2.1 g. of salt, m.p. 186°-188° .
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04032639 |
| Source dataset | uspto-grants-1977_06 |
| ORD ID | ord-750dd0422c6a4e77a9d8f864237df011 |
| Source note | uspto-grants-1977_06 |