HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-Methyl-3-(trifluoromethyl)-4,5-dihydro-1H-pyrazole-4-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 67339313 | HCID 67339313 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 1-Methyl-3-(trifluoromethyl)-4,5-dihydro-1H-pyrazole-4-carboxylic acid | HCID 67340088 | — |
Reaction Steps
1-Methyl-3-trifluoromethyl-4,5-dihydro-1H-pyrazole-4-carboxylic acid ethyl ester (20 g, 90 mmol) was dissolved in 400 ml of dioxan. 400 ml of a 1 N aqueous sodium hydroxide solution (0.4 mol) were added and the reaction mixture was stirred for 2 h at room temperature. Subsequently the mixture was acidified with concentrated hydrochloric acid (pH 2). The dioxan was removed in vacuo, the residue was extracted with ethyl acetate. The combined organic layer was washed with brine, dried over magnesium sulfate and evaporated, delivering 15 g of 1-methyl-3-trifluoromethyl-4,5-dihydro-1H-pyrazole-4-carboxylic acid, which could be directly used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08003626B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-a327e625aeff4945842a4b7e3be99e29 |
| Source note | uspto-grants-2011_08 |