HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Sulfate → 3-Amino-8-t-butyl-1-oxaspiro(4,5)-decane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 86750119 | HCID 86750119 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-Amino-8-t-butyl-1-oxaspiro(4,5)-decane | HCID 19040163 | 76.6% |
Reaction Steps
8-t-Butyl-1-oxaspiro(4,5)-decane-3-one oxime (17.5 g, 76 mmol) in tetrahydrofuran (50 ml) was added to a solution of lithium- aluminium hydride (4.5 g, 0.125 mol) in tetrahydrofuran (100 ml). The reaction mixture was refluxed for 4 hours, cooled end excess LAH was hydrolysed by addition of saturated aqueous sodium sulfate. solids were filtered off washed with tetrahydrofuran and the solvent was stripped off in vacuo. Kugelrohr distillation of the resulting pale yellow oil (16.9 g) gave a colourless oil (12.3 g) Bp.: 125° C./0.02 mbar, nD22 :1.4840.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05591741 |
| Source dataset | uspto-grants-1997_01 |
| ORD ID | ord-913d502fa58b48bdb6c8b03c29b3ab54 |
| Source note | uspto-grants-1997_01 |