HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane → 2,9-Dimethyl-1,2,3,4,5,6-hexahydroazepino[4,3-b]indole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | 9-methyl-2,3,4,5-tetrahydroazepino[4,3-b]indol-1(6H)-one | HCID 28744194 | — |
| Product | 2,9-Dimethyl-1,2,3,4,5,6-hexahydroazepino[4,3-b]indole | HCID 24899050 | — |
Reaction Steps
Lithium aluminum hydride (3 g, 78.95 mmol) was placed in 1,4-dioxane (100 mL) under inert atmosphere and 9-methyl-2,3,4,5-tetrahydroazepino[4,3-b]indol-1(6H)-one (3 g, 14.018 mmol) was added, and the mixture heated to reflux for 15 h. The reaction was monitored by TLC. The reaction was quenched with saturated aqueous sodium sulfate at 0° C., and the reaction mixture filtered. The filtrate was dried over anhydrous sodium sulfate and evaporated to dryness to afford solid, which was washed with water followed by EtOAc, and dried to afford 1.25 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09433626B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-13bddc8cdb4744b6adca3a3f2e2664b0 |
| Source note | uspto-grants-2016_09 |