HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → 6-Methoxy-4,4-dimethyl-1,2,3,4-tetrahydroisoquinoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 69548400 | HCID 69548400 | — |
| Product | 6-Methoxy-4,4-dimethyl-1,2,3,4-tetrahydroisoquinoline | HCID 12283208 | 100% |
Reaction Steps
A solution of 6-methoxy-4,4-dimethyl-1,2,3,4-tetrahydro-isoquinoline-1-one (Intermediate 17, 3.5 g, 17 mmol) in 100 mL of anhydrous tetrahydrofuran was treated with lithium aluminum hydride (1.3 g, 34.25 mmol) in small portions and the resulting suspension was refluxed for 3 hours under argon. The reaction mixture was then cooled in an ice bath and cautiously quenched with saturated aqueous sodium sulfate solution and the resulting slurry was filtered and the filter-cake washed well with ethyl acetate. The filtrate and washings were evaporated in vacuo to a brown oil which was dissolved in chloroform, the solution was dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo to afford the title compound (3.2 g, ˜100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06380256B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-bc95b59c15dc40ba97389873cf4d8807 |
| Source note | uspto-grants-2002_04 |