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Hydrochloric Acid → 1-Chloro-4-hydroxyisoquinoline-3-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Chloro-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester | HCID 86014502 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Chloro-4-hydroxyisoquinoline-3-carboxylic acid | HCID 11020520 | 90% |
反応手順
A mixture of 9.23 g of 1-chloro-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester (33 mmol), 90 ml of 2.5N aqueous sodium hydroxide solution, water (20 ml) and ethanol (110 ml) was refluxed with stirring for 2 h. Then the pH of the mixture was adjusted to 2 by the addition of concentrated aqueous hydrochloric acid. During the addition, the temperature of the mixture was kept at 20° C. by cooling with an ice bath. Stirring was then continued for 1 h before the solid component was separated by vacuum filtration. The filter cake was washed with water and dried in vacuo at 85° C. to give a white powder. 6.64 g of the title compound were obtained; MS-(+)-ion: M+1=224.1 amu.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863292B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-ed749d4451a34ef3a19bf507d693f7ce |
| 出典メモ | uspto-grants-2011_01 |