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Water → 3-chloro-1-methyl-1H-pyrazole-5-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Methyl 3-chloro-1-methyl-1H-pyrazole-5-carboxylate | HCID 67209478 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-chloro-1-methyl-1H-pyrazole-5-carboxylic acid | HCID 18970459 | 91% |
反応手順
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]
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08742106B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-183ac1dfd9d94eadbac3b6ccbdf198fd |
| 出典メモ | uspto-grants-2014_06 |