HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178449165, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tert-Butylamine | HCID 6385 | — |
| Reactant | 4-((3-(3-Chlorophenyl)imidazo[1,2-b]pyridazin-6-yl)amino)cyclohexanone | HCID 71227728 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178449165 | HCID 178449165 | — |
Reaction Steps
To a 0° C. solution of 4-((3-(3-chlorophenyl)imidazo[1,2-b]pyridazin-6-yl)amino)cyclohexanone (80 mg, 0.23 mmol) and t-Butylamine (17.2 mg, 0.23 mmol) in CH2Cl2 (1.2 mL) was added dropwise Ti(Oi-Pr)4 (0.27 mL, 0.92 mmol). The resulting mixture was stirred at room temperature overnight. LCMS showed the reaction was complete. The mixture was poured into water (150 mL) and extracted with EtOAc (100 mL*3). The organic layers were dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by prep. HPLC to give EX. 8-78 (15 mg, 16.5%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09416132B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-099a89e9a3864606bd67e3fe61bf64c1 |
| Source note | uspto-grants-2016_08 |