Sodium hydride → 1-(4-Methylpyridin-3-yl)imidazolidin-2-one
反応式
Cl[CH2:2][CH2:3][NH:4][C:5]([NH:7][C:8]1[CH:9]=[N:10][CH:11]=[CH:12][C:13]=1[CH3:14])=[O:6].[H-].[Na+]>CN(C=O)C.C1COCC1>[CH3:14][C:13]1[CH:12]=[CH:11][N:10]=[CH:9][C:8]=1[N:7]1[CH2:2][CH2:3][NH:4][C:5]1=[O:6]参加物
5
実験手順
1-(2-Chloro-ethyl)-3-(4-methyl-pyridin-3-yl)-urea (I-14a: 8.5 g, 39.96 mmol) in dry DMF (150 mL) was added to a stirred mixture of sodium hydride (2.87 g, 59.94 mmol) in THF (150 mL) at 0° C. The reaction temperature was maintained at room temperature for 30 minutes. The reaction was monitored by TLC. The reaction mixture was quenched with MeOH at 0° C., concentrated under reduced pressure and partitioned between ice water and chloroform. The organic layer was dried over Na2SO4, and concentrated under reduced pressure to afford 6.5 g (91% yield) of 1-(4-methyl-pyridin-3-yl)-imidazolidin-2-one.
後処理
- customThe reaction mixture was quenched with MeOH at 0° C.
- concentrationconcentrated under reduced pressure
- custompartitioned between ice water and chloroform
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-e121337205f84b488c01f8c056573960
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- USRE045173E1
反応ノート
読み込み中…