Water → HCID 178432777、化合物
反応式
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3]([NH2:5])=[NH:4].C(=O)([O-])[O-].[K+].[K+].[Cl:14][CH:15]([C:21]([CH3:23])=O)[C:16](OCC)=[O:17].O>C1CCCCC1>[Cl:14][C:15]1[C:16]([OH:17])=[N:4][C:3]([C:2]([Cl:7])([Cl:6])[Cl:1])=[N:5][C:21]=1[CH3:23]参加物
6
実験手順
A mixture of 30.0 g (0.18 mole) trichloroacetamidine, 25.2 g (0.18 mole) potassium carbonate, 30.3 g (0.18 mole) ethyl 2-chloroacetoacetate, and 300 ml water was stirred 18 hours. The aqueous solution was decanted from heavier tars and acidified with hydrochloric acid. The precipitate that was formed was filtered, washed, and dried to give 14.7 g (31% yield; mp 130°-145° C.) of crude product. An analytical sample was prepared by recrystallization from cyclohexane (mp 156°-157° C.). The structure was confirmed via infrared and elemental analysis.
後処理
- customThe aqueous solution was decanted from heavier tars
- customThe precipitate that was formed
- filtrationwas filtered
- washwashed
- customdried
- customto give 14.7 g (31% yield; mp 130°-145° C.) of crude product
出典と根拠
- ORDレコード
- ord-7fb745fa041a43c0a7da70058a57baa0
- 出典データセット
- uspto-grants-1982_10
- 特許番号
- US04352806
反応ノート
読み込み中…