HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → Tert-butyl 4-[2-(4-fluorophenyl)imidazo[1,2-b]pyridazin-6-yl]piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | 2-Dimethylaminopyridine | HCID 21885 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59406970 | HCID 59406970 | — |
| Product | Tert-butyl 4-[2-(4-fluorophenyl)imidazo[1,2-b]pyridazin-6-yl]piperazine-1-carboxylate | HCID 59406962 | 97% |
Reaction Steps
To a solution of 21.5 g (72.3 mmol) of 2-(4-fluorophenyl)-6-piperazin-1-ylimidazo[1,2-b]pyridazine and 0.44 g (3.6 mmol) of dimethylaminopyridine in 500 mL of chloroform is added dropwise a solution of tert-butyl anhydride dissolved in 100 mL of chloroform. After stirring for 30 minutes at room temperature, the medium is poured into saturated aqueous sodium hydrogen carbonate solution. The organic phase obtained is washed with water, dried over sodium sulfate and then concentrated under reduced pressure to give a brown solid. Finally, 28.0 g of a beige-colored powder are isolated after trituration in a mixture of 200 mL of diisopropyl ether and 10 mL of isopropanol at reflux, followed by cold filtration and drying.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846676B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-b7906541942741acb92f950b19c21b7a |
| Source note | uspto-grants-2014_09 |