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Methanol → 1-(3-chloro-2-pyridinyl)-3-methyl-1H-pyrazole-5-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | ethyl 1-(3-chloro-2-pyridinyl)-3-methyl-1H-pyrazole-5-carboxylate | HCID 66854396 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(3-chloro-2-pyridinyl)-3-methyl-1H-pyrazole-5-carboxylic acid | HCID 66853849 | 89.4% |
反応手順
A mixture of 0.30 g of ethyl 1-(3-chloro-2-pyridinyl)-3-methyl-1H-pyrazole-5-carboxylate, 5 ml of methanol and 5 ml of a 2N aqueous sodium hydroxide solution was heated to reflux for 3 hours. After the reaction mixture was allowed to cool, water was poured and the aqueous layer was washed with methyl t-butyl ether two times. The aqueous layer was adjusted to around pH 3 by an addition of 2N hydrochloric acid, and then extracted with methyl t-butyl ether three times. The combined organic layer was washed with an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 0.24 g of 1-(3-chloro-2-pyridinyl)-3-methyl-1H-pyrazole-5-carboxylic acid of the formula:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07968573B2 |
| 出典データセット | uspto-grants-2011_06 |
| ORD ID | ord-6bcc109377424b11a1757ddb24f8d729 |
| 出典メモ | uspto-grants-2011_06 |