HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 59149740, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 67341254 | HCID 67341254 | — |
| Product | HCID 59149740 | HCID 59149740 | 48.8% |
Reaction Steps
A stirred solution of methyl 2-[[1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]methoxy]acetate (95 mg, 0.25 mmol) in 2M dimethylamine in methanol (2.0 mL, 4.00 mmol) was heated at 120° C. in a microwave reactor for 1 hour. The reaction mixture was evaporated and the crude product was purified by preparative LCMS (Waters XBridge Prep C18 OBD column, 5μ silica, 19 mm diameter, 100 mm length), using decreasingly polar mixtures of water (containing 1% ammonia) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford N,N-dimethyl-2-[[1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]methoxy]acetamide (48.0 mg, 48.8%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08003649B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-58b709e056dc4dc2bcaf3b810b2c10c9 |
| Source note | uspto-grants-2011_08 |