HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 68432135, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Stannous chloride dihydrate | HCID 61436 | — |
| Reactant | HCID 68432095 | HCID 68432095 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68432135 | HCID 68432135 | 43.1% |
Reaction Steps
2-[5-Bromo-3-nitro-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 (32 mg, 0.0616 mmol) in ethyl acetate (3 mL) was stirred with tin (II) chloride dihydrate (72 mg, 0.319 mmol) at room temperature for 2 hours. After completion of the reaction, the reaction solution was basified to pH 9-10 with aqueous sodium hydroxide and filtered through celite. The filtrate was extracted with ethyl acetate, and the extract was dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform/methanol=6/1) to give the desired product (13 mg, 43% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08440666B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-67b7c751622345ed9b766efe743b5026 |
| Source note | uspto-grants-2013_05 |