HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 10131987, compound → HCID 22605936, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 10131987 | HCID 10131987 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22605936 | HCID 22605936 | — |
Reaction Steps
A solution of N-[4-(3,4-dihydro-1H-isoquinolin-2-yl)-6-methyl-pyridin-2-yl]-oxalamic acid ethyl ester (example 33) (0.43 g, 1.3 mmol) in THF (20 ml) was cooled in an ice bath and lithium aluminum hydride (0.12 g, 3.2 mmol) was added in. The mixture was stirred at rt for 2 hr, quenched with saturated aqueous Seignette-salt solution and filtered. The organic phase was dried (Na2SO4) and concentrated. After chromatograpy (SiO2 with CH2Cl/CH3OH/NH4OH=200/10/1) the title compound was obtained as a colorless oil (0.18 g, 47%). Mp. 160-162° C. (AcOEt), MS: m/e=296(M−H−).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06831087B2 |
| Source dataset | uspto-grants-2004_12 |
| ORD ID | ord-73153206329e4e3daec73fa3ccacdbf2 |
| Source note | uspto-grants-2004_12 |