反応式
[CH2:1]([NH:3][C:4]1[C:9]([CH:10]=O)=[CH:8][N:7]=[C:6]([S:12][CH3:13])[N:5]=1)[CH3:2].CO[C:16]1[CH:17]=[C:18]([CH2:24][C:25]#[N:26])[CH:19]=[C:20]([O:22][CH3:23])[CH:21]=1.[C:27]([O-:30])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:23][O:22][C:20]1[CH:19]=[C:18]([C:24]2[C:25](=[NH:26])[N:3]([CH2:1][CH3:2])[C:4]3[N:5]=[C:6]([S:12][CH3:13])[N:7]=[CH:8][C:9]=3[CH:10]=2)[CH:17]=[C:16]([O:30][CH3:27])[CH:21]=1参加物
5
実験手順
To a solution of the product of Example 3, 4-ethylamino-2-methylsulfanyl-pyrimidine-5-carboxaldehyde (37.0 g, 0.19 mol) and 3,5-dimethoxyphenylacetonitrile (37.0 g, 0.21 mol) in DMF (300 mL) was added portionwise anhydrous K2CO3 (130 g) with stirring. The reaction mixture was heated overnight at 105–110° C. and filtered hot. The insoluble salts were washed with DMF (100 mL), and water was added to the warm filtrate until the solution just turned turbid. Crystals developed upon seeding or inducement (scratching with a glass rod). The product was collected by filtration, washed with 100 mL DMF/H2O (25:75), washed with water, and dried in vacuo to afford 50.5 g (76%) of the titled compound. mp 93–95° C.
後処理
- temperatureThe reaction mixture was heated overnight at 105–110° C.
- filtrationfiltered hot
- washThe insoluble salts were washed with DMF (100 mL), and water
- additionwas added to the warm filtrate until the solution just turned turbid
- filtrationThe product was collected by filtration
- washwashed with 100 mL DMF/H2O (25:75)
- washwashed with water
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-b253223e501e42c8b794043a5caa9902
- 出典データセット
- uspto-grants-2006_04
- 特許番号
- US07022711B2
関連ノート
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