Hydrochloric Acid → 3-Oxo-3-(thiophen-3-yl)propanenitrile
反応式
N[C:2]([C:6]1[CH:10]=[CH:9][S:8][CH:7]=1)=[CH:3][C:4]#[N:5].Cl.C[OH:13]>>[O:13]=[C:2]([C:6]1[CH:10]=[CH:9][S:8][CH:7]=1)[CH2:3][C:4]#[N:5]参加物
4
実験手順
A 1.2 g. portion of β-amino-3-thiopheneacrylonitrile is added to 10 ml. of 1 N hydrochloric acid. A 40 ml. portion of methanol is added and the mixture is stirred for 3 hours. The mixture is evaporated in vacuo to a residue which is dissolved in 35 ml. of hot methanol and treated with charcoal. After cooling, petroleum ether is added, the mixture is filtered and the collected solid is discarded. The filtrate is evaporated and the residue is dissolved in 35 ml. of hot isopropanol and the insoluble material is filtered and discarded. The filtrate is cooled and the solid is collected giving the desired products as white plates, mp. 87°-88° C.
後処理
- customThe mixture is evaporated in vacuo to a residue which
- dissolutionis dissolved in 35 ml
- additionof hot methanol and treated with charcoal
- temperatureAfter cooling
- additionpetroleum ether is added
- filtrationthe mixture is filtered
- customThe filtrate is evaporated
- dissolutionthe residue is dissolved in 35 ml
- filtrationof hot isopropanol and the insoluble material is filtered
- temperatureThe filtrate is cooled
- customthe solid is collected
出典と根拠
- ORDレコード
- ord-af28c428355f491bb51822c43707b914
- 出典データセット
- uspto-grants-1982_09
- 特許番号
- US04350689
反応ノート
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