Water → 1-Tert-butyl-3-(3-oxo-1-cyclohexene-1-yl)urea
反応式
[C:1]1(=O)[CH2:6][CH2:5][CH2:4][C:3](=[O:7])[CH2:2]1.[C:9]([NH:13][C:14]([NH2:16])=[O:15])([CH3:12])([CH3:11])[CH3:10].O>C1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:9]([NH:13][C:14]([NH:16][C:1]1[CH2:6][CH2:5][CH2:4][C:3](=[O:7])[CH:2]=1)=[O:15])([CH3:12])([CH3:11])[CH3:10]参加物
6
実験手順
To a solution of 11.2 g of 1,3-cyclohexanedione in 250 ml of benzene is added 11.6 g tert-butylurea and 100 mg of p-toluenesulfonic acid. The solution is heated at reflux under nitrogen with water removal for three hours. At the end of this period the solution is cooled and the precipitated product removed by filtration. The precipitate is recrystallized from acetonitrile to give 14 g of 1-tert-butyl-3-(3-oxo-1-cyclohexene-1-yl)urea, m.p. 223°-225° C.
後処理
- temperatureThe solution is heated
- temperatureAt the end of this period the solution is cooled
- customthe precipitated product removed by filtration
- customThe precipitate is recrystallized from acetonitrile
出典と根拠
- ORDレコード
- ord-8431755f137a43b69ed8b570e3c7ee3b
- 出典データセット
- uspto-grants-1977_01
- 特許番号
- US04002767
反応ノート
読み込み中…