Potassium Carbonate → 8-Chloro-3,4-dihydro-1H-pyrimido[1,6-A]pyrimidin-6(2H)-one
反応式
Br[CH2:2][CH2:3][CH2:4][NH:5][C:6]1[CH:11]=[C:10]([Cl:12])[N:9]=[C:8](Cl)[N:7]=1.C(=O)([O-])[O-:15].[K+].[K+]>O1CCOCC1.O>[Cl:12][C:10]1[CH:11]=[C:6]2[NH:5][CH2:4][CH2:3][CH2:2][N:7]2[C:8](=[O:15])[N:9]=1参加物
5
反応条件
- 温度
- 60 °C
実験手順
A suspension of N-(3-bromopropyl)-2,6-dichloropyrimidin-4-amine (47 g, 165 mmol) and potassium carbonate (68.4 g, 495 mmol) in 1,4-dioxane (100 mL) and water (100 mL), was heated to 60° C. overnight. The mixture was evaporated to remove the dioxane solvent and the mixture was adjusted to pH ˜6 with HCl (6M). The mixture was extracted with ethyl acetate to remove by product and aqueous phase was adjusted to pH ˜7 with NaOH (2M), evaporated to afford the title compound (17 g, 55% yield).
後処理
- customThe mixture was evaporated
- customto remove the dioxane solvent
- extractionThe mixture was extracted with ethyl acetate
- customto remove by product and aqueous phase
- customevaporated
出典と根拠
- ORDレコード
- ord-363685049e044985bc56aceed9d34aa9
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09273054B2
反応ノート
読み込み中…