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
To a solution of N-(3-bromopropyl)-2,6-dichloropyrimidin-4-amine (2.0 g, 7.02 mmol) in 1,4-dioxane (15 mL) and water (15 mL) was added potassium carbonate (2.0 g, 14.47 mmol), stirred for 2 h at 60° C. and then concentrated. The residue was neutralized to pH˜6 by hydrochloride solution (6M), extracted by ethyl acetate to remove byproduct, and then neutralized by sodium hyroxide (2M) to pH˜7. The water was removed in vacuum to afford the title compound (3.03 g).
後処理
- concentrationconcentrated
- extractionextracted by ethyl acetate
- customto remove byproduct
- customThe water was removed in vacuum
出典と根拠
- ORDレコード
- ord-c5de83f88cb348d88166c44d32445a81
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296755B2
反応ノート
読み込み中…