HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 1-Methyl-1,2,3,4-tetrahydroisoquinoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 1-Methylisoquinoline | HCID 15592 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Methyl-1,2,3,4-tetrahydroisoquinoline | HCID 92214 | 77% |
Reaction Steps
To a solution of 1-methylisoquinoline (133 μL, 1.0 mmol) in THF under nitrogen was added dropwise a solution of LiBEt3H in THF (1.0M, 2.2 mL, 2.2 mmol) to give a yellow solution. After stirring 1.5 h, MeOH (1.2 mL) was added dropwise to produce a clear colorless solution, which was then diluted with 1M aq. HCl and ether. The aqueous layer was extracted three times with ether, then made basic (pH 14) by addition of 1M aq. NaOH. The aqueous layer was extracted five times with DCM, dried over MgSO4, filtered and concentrated to give the desired product in 77% yield, which was used without further purification. LC/MS (10-99%) M/Z: M+1 obs=148.3; tR=0.62 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08202861B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-fdfd77e7568a4b23875f7459fee22714 |
| Source note | uspto-grants-2012_06 |