HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 3-chloro-1-methyl-1H-pyrazole-5-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | Methyl 3-chloro-1-methyl-1H-pyrazole-5-carboxylate | HCID 67209478 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 3-chloro-1-methyl-1H-pyrazole-5-carboxylic acid | HCID 18970459 | 91% |
Reaktionsschritte
To a solution of methyl 3-chloro-1-methyl-1H-pyrazole-5-carboxylate (6.0 g, 34.4 mmol) in dioxane (10 ml) was added H2O (10 ml) and LiOH (1.65 g, 68.7 mmol). After stirring for 16 h, the reaction mixture was washed with CH2Cl2 and then the aqueous phase acidified by drop wise addition of conc. HCl. The resulting residue was filtered off, washed with water and dried to yield the title compound (5.0 g, 91%). [1H-NMR (DMSO-d6, 360 MHz) δ 13.77 (br. s, 1H), 6.88 (d, 1H), 4.05 (s, 3H); HPLC-MS RtJ=0.47 min; [M+H]+=160.9, 163.0]
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08742106B2 |
| Quelldatensatz | uspto-grants-2014_06 |
| ORD ID | ord-183ac1dfd9d94eadbac3b6ccbdf198fd |
| Quellennotiz | uspto-grants-2014_06 |