Hydrochloric Acid → 3-chloro-1-methyl-1H-pyrazole-4-carboxylic acid
反応式
[Cl:1][C:2]1[C:6]([C:7]([O:9]CC)=[O:8])=[CH:5][N:4]([CH3:12])[N:3]=1.[OH-].[Na+].Cl>O>[Cl:1][C:2]1[C:6]([C:7]([OH:9])=[O:8])=[CH:5][N:4]([CH3:12])[N:3]=1参加物
5
実験手順
A mixture of 23.9 g (127 mmol) of ethyl 3-chloro-1-methylpyrazole-4-carboxylate and 10.4 g (260 mmol) of sodium hydroxide in 130 mL of water was prepared and was heated at reflux for 3 hr. The solution that formed was cooled to about 0° C. and neutralized to pH 6.5 with concentrated hydrochloric acid with stirring and the precipitate that formed was recovered by filtration, washed with water, and dried under reduced pressure to obtain 18.1 g (89 percent of theory) of the title compound as a white solid melting at 211°-213° C. (d).
後処理
- customwas prepared
- temperaturewas heated
- temperatureat reflux for 3 hr
- customThe solution that formed
- customthe precipitate that formed
- filtrationwas recovered by filtration
- washwashed with water
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-a43bcfea1fad456abf591cdcb87617ea
- 出典データセット
- uspto-grants-1993_04
- 特許番号
- US05201938
反応ノート
読み込み中…