反応式
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[S:10][CH:9]=[C:8]([CH3:11])[C:6]=2[N:7]=1.[CH3:13][CH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>CN(C=O)C>[Cl:1][C:2]1[N:3]=[C:4]([N:17]2[CH2:18][CH2:19][CH:14]([CH3:13])[CH2:15][CH2:16]2)[C:5]2[S:10][CH:9]=[C:8]([CH3:11])[C:6]=2[N:7]=1参加物
反応条件
- 温度
- 0 °C
実験手順
In 10 ml of DMF was dissolved 1.0 g (4.6 mmol) of 2,4-dichloro-7-methylthieno[3,2-d]pyrimidine, and then 1.06 g (10.7 mmol) of 4-methylpiperidine was added dropwise to the resulting solution under ice cooling over 5 minutes. The reaction mixture was stirred at 0° C. for one hour and then allowed to resume to room temperature, followed by stirring for one hour. After completion of the reaction, ice water was added to the reaction mixture, followed by extraction with ethyl acetate (50 ml×3). After the organic layer was washed successively with 1N hydrochloric acid, water and brine and dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/10) to give 1.20 g (yield: 93.3%) of the title compound.
後処理
- customto resume to room temperature
- stirringby stirring for one hour
- additionwas added to the reaction mixture
- extractionfollowed by extraction with ethyl acetate (50 ml×3)
- washAfter the organic layer was washed successively with 1N hydrochloric acid, water and brine
- dry with materialdried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/10)
出典と根拠
- ORDレコード
- ord-64ecb0c4f947486599238ad569b6f601
- 出典データセット
- uspto-grants-2002_01
- 特許番号
- US06339089B2
関連ノート
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