HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 66935818, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 3-Pentanol | HCID 11428 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86650802 | HCID 86650802 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66935818 | HCID 66935818 | — |
Reaction Steps
3-Pentanol (1.2 ml) was initially charged at RT with stirring. Thereafter, sodium hydride (77 mg) was added while cooling with ice. After stirring at 55° C. for 3 h, (6-chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylamine (W2.169; 50 mg), dissolved in 3-pentanol (1 ml) and DMF (2 ml), was added dropwise. After stirring for 2 h, the reaction mixture was left to stand at RT overnight, admixed with water and dichloromethane and then extracted three times more with dichloromethane. The combined organic phases were dried over magnesium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. 44 mg of the title compound were obtained. LC-MS rt: 0.86 min [M+H]+: 264.2 (met. b)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08198272B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-de56b59ef54b422582f5dde621091aa1 |
| Source note | uspto-grants-2012_06 |