HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68432076, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 68431201 | HCID 68431201 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68432076 | HCID 68432076 | 25% |
Reaction Steps
2-(5-Chloro-6-oxo-4-{[(1R,2R,3R,5S)-2,6,6-trimethylbicyclo[3.1.1]hept-3-yl]amino}pyridazin-1(6H)-yl)-N-(pyridin-4-ylmethyl)acetamide (40 mg, 0.0873 mmol) was added to lithium aluminum hydride (4.3 mg, 0.104 mmol) in tetrahydrofuran (1 mL) at 0° C., and the resulting reaction solution was stirred at room temperature for 1.5 hours. After completion of the reaction, the reaction solution was mixed with water, ethyl acetate and anhydrous magnesium sulfate and filtered, and the filtrate was evaporated under reduced pressure. The resulting residue was purified by preparative thin layer chromatography (chloroform/methanol=13/1) to give the desired product (9.5 mg, 25% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08440666B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-de60c616c71646d5b4fb226fd965c25a |
| Source note | uspto-grants-2013_05 |