反応式
[CH2:1]([NH:4][C:5]([NH2:7])=[O:6])[CH:2]=[CH2:3].[CH:8](=[O:12])/[CH:9]=[CH:10]/[CH3:11].[CH3:13][CH2:14]O>Cl>[CH2:1]([N:4]1[CH:8]([O:12][CH2:13][CH3:14])[CH2:9][CH:10]([CH3:11])[NH:7][C:5]1=[O:6])[CH:2]=[CH2:3]参加物
実験手順
Following a related procedure, [G. Zigeuner, W. Rauter, Monatshefte fur Chemie, 96, 1950 (1965)], allylurea (24.5 g, 0.25 mol), crotonaldehyde (19.67 g, 0.29 mol) and 37% HCl (12 drops) were mixed with 140 g of EtOH at room temperature for 3d, during which all of the crotonaldehyde was consumed. The major product had a retention time near that of allylurea. The dark mixture was neutralized with Na2CO3, filtered and concentrated at reduced pressure. Part of the crude mixture was extracted with cyclohexane, decolorized with charcoal, filtered and concentrated to give a light yellow oil which produced white crystals (mp 72°-76° C.) on standing. A separate sample was submitted to kugelrohr distillation (0.05 torr) to give further products: E at 90° C., F at 145°-155° C. (solid, mp 72°-76° C.) and G at 145°-155° C. (liquid).
後処理
- customwas consumed
- filtrationfiltered
- concentrationconcentrated at reduced pressure
- extractionPart of the crude mixture was extracted with cyclohexane
- filtrationfiltered
- concentrationconcentrated
- customto give a light yellow oil which
出典と根拠
- ORDレコード
- ord-ec717c1fb8ff42f0bad35b17e9488a59
- 出典データセット
- uspto-grants-1989_09
- 特許番号
- US04864055
関連ノート
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