反応式
[Na].[NH2:2][C:3]([NH2:5])=[S:4].[C:6]([C:8]([C:20]#[N:21])=[CH:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:19])[CH3:18])=[CH:12][CH:11]=1)#[N:7]>C(O)C>[NH2:21][C:20]1[C:8]([C:6]#[N:7])=[C:9]([C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:19])[CH3:18])=[CH:12][CH:11]=2)[NH:2][CH:3]([SH:4])[N:5]=1参加物
実験手順
To 20 mL of absolute ethanol, 250 mg of metallic sodium was added in small portions. After dissolved completely, 760 mg of thiourea was added to the above solution, and the mixture was stirred at room temperature for 1 hour. To the reaction, 2.11 g of N-[4-(2,2-dicyanovinyl)phenyl]acetamide was added, and the mixture was heated to reflux for 3 hours. Then, the solvent was removed under reduced pressure from the reaction mixture, the residue was dissolved in 30 mL of water. In addition, the mixture was acidified by adding acetic acid in small portions, thereto 30 mL of ethyl acetate was added and then the solution was stirred overnight. Filtration of the precipitated material gave 1.2 g of N-[4-(6-amino-5-cyano-2-mercapto-2,3-dihydropyrimidin-4-yl)phenyl]acetamide as a white powder.
後処理
- dissolutionAfter dissolved completely
- additionwas added
- temperaturethe mixture was heated
- temperatureto reflux for 3 hours
- customThen, the solvent was removed under reduced pressure from the reaction mixture
- dissolutionthe residue was dissolved in 30 mL of water
- additionby adding acetic acid in small portions
- addition30 mL of ethyl acetate was added
- stirringthe solution was stirred overnight
- filtrationFiltration of the precipitated material
出典と根拠
- ORDレコード
- ord-283d8ec913ef41e3a40018170ed5eefd
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07989446B2
関連ノート
読み込み中…