Water → HCID 21114633、化合物
反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([F:9])=[CH:4][N:3]=1.C(N(CC)CC)C.[C:17]([NH2:20])#[C:18][CH3:19].O>C(#N)C>[Cl:1][C:2]1[N:7]=[C:6]([NH:20][CH2:17][C:18]#[CH:19])[C:5]([F:9])=[CH:4][N:3]=1参加物
6
実験手順
11.1 g (66 mmol) of 2,4-dichloro-5-fluoropyrimidine is dissolved in 60 ml of acetonitrile, and 10.2 ml (73 mmol) of triethylamine and 6.0 ml (86 mmol) of propynylamine are added. The reaction mixture is stirred overnight at room temperature and then poured into water. The mixture is extracted by means of ethyl acetate, the combined organic phases are dried on MgSO2, and the solvent is evaporated by means of underpressure. After the remaining material is recrystallized with diisopropyl ether/hexane, the yield is 10.6 g (87% of theory) of the product.
後処理
- extractionThe mixture is extracted by means of ethyl acetate
- customthe combined organic phases are dried on MgSO2
- customthe solvent is evaporated by means of underpressure
- customAfter the remaining material is recrystallized with diisopropyl ether/hexane
出典と根拠
- ORDレコード
- ord-bd6bdb235b7b43f09b4b6256ad72f9ad
- 出典データセット
- uspto-grants-2009_10
- 特許番号
- US07598260B2
反応ノート
読み込み中…