HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 3-(1-Methanesulfonylpiperidin-3-yl)-6-piperidin-1-yl-1,2,4-triazolo[4,3-b]pyridazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 6-Piperidin-1-yl-3-piperidin-3-yl-1,2,4-triazolo[4,3-b]pyridazine | HCID 23057946 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(1-Methanesulfonylpiperidin-3-yl)-6-piperidin-1-yl-1,2,4-triazolo[4,3-b]pyridazine | HCID 23057962 | 27% |
Reaction Steps
To a solution mixture of 6-piperidin-1-yl-3-piperidin-3-yl-1,2,4-triazolo[4,3-b]pyridazine (670 mg), triethylamine (360 mg) and methylene chloride (15 ml), methanesulfonyl chloride (320 mg) was added and the mixture was stirred at room temperature for 8 hours. The reaction solution was concentrated under reduced pressure, and the resultant residue was extracted with ethyl acetate. The extract was washed successively with water and brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resultant crude crystals were recrystallized from ethanol to obtain 3-(1-methanesulfonylpiperidin-3-yl)-6-piperidin-1-yl-1,2,4-triazolo[4,3-b]pyridazine (230 mg) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07173033B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-54a8e83216f44d0e9bb2fa0427ef1e2f |
| Source note | uspto-grants-2007_02 |