Piperazine → 4-Chloro-6-(piperazin-1-yl)pyrimidine hydrochloride
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.[NH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1>C(#N)C>[ClH:1].[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:7]=1参加物
4
反応条件
- 温度
- 2.5 °C
実験手順
A solution of 14.8 g of 4,6-dichloropyrimidine in 100 ml of acetonitrile is cooled to 0-5° C., a solution of 20 g of anhydrous piperazine in 200 ml of acetonitrile is added over 30 minutes and the mixture is left with stirring at 0-5° C. for 2 hours. It is concentrated under vacuum, the residue is taken up with 100 ml of 2N NaOH and extracted with ether, the organic phase is dried over Na2SO4 and the solvent is evaporated under vacuum. The hydrochloride is formed, giving 15 g of the expected product.
後処理
- waitthe mixture is left
- concentrationIt is concentrated under vacuum
- extractionextracted with ether
- dry with materialthe organic phase is dried over Na2SO4
- customthe solvent is evaporated under vacuum
出典と根拠
- ORDレコード
- ord-f6a0cefb2a014cd68ce8c899835c8e0d
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07468368B2
反応ノート
読み込み中…