HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → 2-(4,5-Dimethylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 1154030-52-0 | HCID 55279158 | — |
| Reactant | 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester | HCID 68704864 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-(4,5-Dimethylpyridin-2-yl)-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one | HCID 59280190 | — |
Reaction Steps
220 mg (1.0 mmol) of the compound from Example 2A are initially charged in 5 ml of ethanol. 137 mg (1.0 mmol) of the compound from Example 21A and 38 mg (0.2 mmol) of p-toluenesulfonic acid are added, and the mixture is stirred under reflux for 16 h. The mixture is then allowed to cool to RT, and the solid formed is filtered off, washed with tert-butyl methyl ether and dried under high vacuum. This gives 28 mg of the title compound. The mother liquor is put aside and used for preparing the hydrochloride (see Example 87).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08609698B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-160c512f588e4d75a9c22877d81ae7f1 |
| Source note | uspto-grants-2013_12 |