HCID 22997467、化合物 → 3-(5-methyl-1H-imidazol-4-yl)propanoic acid hydrochloride
反応式
[ClH:1].[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1/[CH:8]=[CH:9]/[C:10]([OH:12])=[O:11].CCCCCCC.C(OC(C)C)(C)C>[Pd].O1CCCC1.O>[ClH:1].[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1[CH2:8][CH2:9][C:10]([OH:12])=[O:11]参加物
5
実験手順
60 mg of palladium-on-charcoal at 10% are added to a solution of 387 mg (1.1 mmol) of (E)-3-(5-methyl-1H-imidazol-4-yl)acrylic acid hydrochloride in a 1/1 tetrahydrofuran/water mixture. The reaction medium is placed under a hydrogen atmosphere and stirred for 19 h, and then filtered through celite. The filtrate is concentrated under vacuum. The residue obtained is taken up in a heptane/diisopropyl ether mixture with stirring for 2 h. The white precipitate formed is filtered off and then dried. 326 mg of 3-(5-methyl-1H-imidazol-4-yl)propanoic acid hydrochloride are obtained in the form of a white solid with a yield of 83%.
後処理
- filtrationfiltered through celite
- concentrationThe filtrate is concentrated under vacuum
- customThe residue obtained
- stirringwith stirring for 2 h
- customThe white precipitate formed
- filtrationis filtered off
- customdried
出典と根拠
- ORDレコード
- ord-61ac989c36b148929a6a478abcb60eba
- 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…