HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane → HCID 178520834, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 178468649 | HCID 178468649 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178520834 | HCID 178520834 | 25% |
Reaction Steps
To a solution of 5-[4-(3-Hydroxy-propylamino)-7-trifluoromethyl-imidazo[1,2-a]quinoxalin-1-yl]-1H-pyrazole-3-carboxylic acid ethyl ester (0.08 mmol; 36 mg), in THF (0.2 mL) under argon cooled to 0° C., was added LAH (0.24 mmol; 10 mg). The reaction was slowly warmed up to room temperature over 4 hr, then to 45° C. overnight. After addition of dioxane (1 mL), the mixture was heated to 75° C. for 24 hr. After quenching with Rochelle's salt, the mixture was extracted with ethyle acetate. The organic phase was dried, concentrated. The residue was purified by preparative TLC (dichloromethane/methanol) to yield the title compound as a white solid (7 mg; 0.02 mmol; 21%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08513250B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-cbe2b925a5284d3692fc358892bf8d4c |
| Source note | uspto-grants-2013_08 |