Sodium Hydroxide → HCID 178433263、化合物
反応式
[CH3:1][C:2]1[N:6]=[CH:5][NH:4][C:3]=1[CH:7]=[CH:8][C:9]([Cl:11])=[O:10].[OH-].[Na+].[H][H]>[Pd]>[CH3:1][C:2]1[N:6]=[CH:5][NH:4][C:3]=1[CH2:7][CH2:8][C:9]([Cl:11])=[O:10]参加物
5
反応条件
- 温度
- 80 °C
実験手順
50 mg of palladium-on-charcoal at 10% are added to 500 mg (2.65 mmol) of 3-(5-methyl-3H-imidazol-4-yl)acrylic acid chloride in 10 ml of a 0.5N solution of sodium hydroxide. The reaction mixture is placed under 6 bar of hydrogen pressure and stirred at 80° C. for 72 hours. After having filtered off the catalyst through celite, the residue is acidified to pH 2 with hydrochloric acid, concentrated to dryness and taken up in ethanol. The insoluble material is filtered off and the filtrate is concentrated to dryness. 102 mg of 3-(5-methyl-3H-imidazol-4-yl)propanoic acid chloride are obtained in the form of a white powder with a yield of 16%.
後処理
- filtrationAfter having filtered off the catalyst through celite
- concentrationconcentrated to dryness
- filtrationThe insoluble material is filtered off
- concentrationthe filtrate is concentrated to dryness
出典と根拠
- ORDレコード
- ord-22909198763949ee8182ca80a00743fa
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08871187B2
反応ノート
読み込み中…