Aniline → Pyrimido(5,4-d)pyrimidine
反応式
NC1C=CC=CC=1.Cl[C:9]1[N:10]=[C:11](Cl)[C:12]2[N:17]=[C:16](Cl)[N:15]=[C:14](Cl)[C:13]=2[N:20]=1>C(Cl)(Cl)Cl>[N:17]1[C:12]2[CH:11]=[N:10][CH:9]=[N:20][C:13]=2[CH:14]=[N:15][CH:16]=1参加物
4
実験手順
8.7 mL (95 mmol) of aniline may be slowly added dropwise to a solution of 4 g (19 mmol) of 2,4,6,8-tetrachloropyrimidopyrimidine in 50 mL of chloroform in a water bath at about 0° C. The results of the reaction may be verified by thin layer chromatography (TLC). The reaction mixture may be washed with an aqueous ammonium chloride solution and extracted with chloroform. The organic layer may be separated, distilled under reduced pressure to remove the solvent, and dried in an oven to yield approximately 5 g of Compound 5a. Compound 5a may be a substantially pale yellow solid.
後処理
- customThe results of the reaction
- washThe reaction mixture may be washed with an aqueous ammonium chloride solution
- extractionextracted with chloroform
- customThe organic layer may be separated
- distillationdistilled under reduced pressure
- customto remove the solvent
- customdried in an oven
出典と根拠
- ORDレコード
- ord-80ecc067189e4267a4fab8d5cf886adf
- 出典データセット
- uspto-grants-2009_12
- 特許番号
- US07632947B2
反応ノート
読み込み中…