4-Bromobutyronitrile → 4-(5-Methyl-4-imidazolylmethylthio)butyronitrile
反応式
[Na].[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1[CH2:8][SH:9].Br[CH2:11][CH2:12][CH2:13][C:14]#[N:15]>C(O)C>[CH3:2][C:3]1[NH:7][CH:6]=[N:5][C:4]=1[CH2:8][S:9][CH2:11][CH2:12][CH2:13][C:14]#[N:15]参加物
5
実験手順
Sodium (5.0 g) was dissolved in ethanol (300 ml) and 5-methyl-4-(mercaptomethyl)imidazole (17 g) added, followed by a solution of 4-bromobutyronitrile (16 g) in ethanol (50 ml). The mixture was stirred under reflux for 45 minutes, cooled, filtered and the filtrate evaporated to dryness. The residue was taken up in water and extracted with ethyl acetate. The extract was dried (MgSO4) and solvent removed. Recrystallisation of the product from ethanol-ether gave 4-(5-methyl-4-imidazolylmethylthio)butyronitrile as its hydrochloride salt (12 g).
後処理
- temperatureunder reflux for 45 minutes
- temperaturecooled
- filtrationfiltered
- customthe filtrate evaporated to dryness
- extractionextracted with ethyl acetate
- dry with materialThe extract was dried (MgSO4) and solvent
- customremoved
- customRecrystallisation of the product from ethanol-ether
出典と根拠
- ORDレコード
- ord-230baa72ed0249c6a3803a7cfa090eb6
- 出典データセット
- uspto-grants-1989_02
- 特許番号
- US04808589
反応ノート
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