Hydrochloric Acid → 2-Acetylamino-3-cyano-4-ethoxy-5-formylthiophene
反応式
[C:1]([NH:4][C:5]1[S:6][CH:7]=[C:8]([O:12][CH2:13][CH3:14])[C:9]=1[C:10]#[N:11])(=[O:3])[CH3:2].P(Cl)(Cl)(Cl)=O.[OH-].[Na+].Cl.CN(C)[CH:25]=[O:26]>>[C:1]([NH:4][C:5]1[S:6][C:7]([CH:25]=[O:26])=[C:8]([O:12][CH2:13][CH3:14])[C:9]=1[C:10]#[N:11])(=[O:3])[CH3:2]参加物
6
実験手順
210 parts of 2-acetylamino-3-cyano-4-ethoxythiophene (Example 7) are introduced into 1000 parts of dimethylformamide, and 200 parts of phosphoryl trichloride are added dropwise in the course of 4 hours. Stirring is continued for 4 hours at 60° C., after which the resulting crystal slurry is brought into solution by adding 600 parts of ice. This solution is stirred into 2000 parts of 12.5% strength sodium hydroxide solution, and acidified with hydrochloric acid after 6 hours. The precipitated product is filtered off under suction, washed with water and dried to give 201 parts of 2-acetylamino-3-cyano-4-ethoxy-5-formylthiophene. A sample recrystallized from dimethylformamide has a melting point of 276°-277° C. and possesses the following analytical values: