Hydrogen Bromide → HCID 49788132、化合物
反応式
[CH2:1]([O:3][C:4](=[O:18])[CH:5]([C:16]#[N:17])[CH2:6][C:7]([C:9]1[CH:14]=[CH:13][N:12]=[C:11]([NH2:15])[N:10]=1)=O)[CH3:2].[BrH:19]>CCOCC.C(Cl)Cl.CC(O)=O>[CH2:1]([O:3][C:4]([C:5]1[CH:6]=[C:7]([C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH2:15])[N:10]=2)[NH:17][C:16]=1[Br:19])=[O:18])[CH3:2]参加物
6
実験手順
A solution of 4-(2-amino-pyrimidin-4-yl)-2-cyano-4-oxo-butyric acid ethyl ester (364 mg, 1.47 mmol) in anhydrous Et2O and DCM (1:1 10 mL) was added dropwise to 4.5 mL of 33% HBr in AcOH at 0° C. The mixture was left at 0° C. for 30 min and then at rt until disappearance of the starting material. The solid was filtered, washed with acetone and MeOH, neutralized with 7N NH3 in MeOH to afford 400 mg (88%) of the title compound.
後処理
- customat rt
- filtrationThe solid was filtered
- washwashed with acetone and MeOH
出典と根拠
- ORDレコード
- ord-5bf71a72427740a0aac3d6cf4f9d826f
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08426417B2
反応ノート
読み込み中…