HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58136921, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 58136934 | HCID 58136934 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | 3-Pentanol | HCID 11428 | — |
| Product | HCID 58136921 | HCID 58136921 | — |
Reaction Steps
3-Pentanol (2.5 ml) was initially charged at RT with stirring. Thereafter, sodium hydride (91 mg) was added while cooling with ice. After stirring at 55° C. for 2.5 h, 6-chloro-7-ethyl-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine (W2.007; 120 mg), dissolved in 3-pentanol (2 ml) and DMF (4 ml), was added dropwise. After stirring for 1 h, the mixture was left to stand at RT overnight, and the reaction mixture was admixed with water and dichloromethane and then extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. 126 mg of the title compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08198272B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-5193005dc181472489104a3a95f3b1c1 |
| Source note | uspto-grants-2012_06 |