Phosphorus oxychloride → Butyl 6-chloropyridazine-3-carboxylate
反応式
P(Cl)(Cl)([Cl:3])=O.O=[C:7]1[NH:12][N:11]=[C:10]([C:13]([O:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:14])[CH:9]=[CH:8]1>C(#N)C.O>[Cl:3][C:7]1[N:12]=[N:11][C:10]([C:13]([O:15][CH2:16][CH2:17][CH2:18][CH3:19])=[O:14])=[CH:9][CH:8]=1参加物
5
実験手順
To a mixture of phosphorus oxychloride (20 ml) and acetonitrile (40 ml) heated at reflux was added a solution of n-butyl 6-oxo-1,6-dihydropyridazine-3-carboxylate (20 g) in acetonitrile (80 ml). The reaction was heated at reflux for 30 minutes, cooled and added to an ice cooled solution of K2C03 (87.8 g) in water (600 ml) with vigorous stirring. The product was filtered off, washed with water and dried at 60° C. to give n-butyl 6-chloropyridazine-3-carboxylate (17.5 g, 80% yield), mpt 110-111° C.
後処理
- temperatureheated
- temperatureat reflux
- temperatureThe reaction was heated
- temperatureat reflux for 30 minutes
- temperaturecooled
- filtrationThe product was filtered off
- washwashed with water
- customdried at 60° C.
出典と根拠
- ORDレコード
- ord-87eff584b3e146b9828cd7e6cb639779
- 出典データセット
- uspto-grants-2000_08
- 特許番号
- US06100258
反応ノート
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