反応式
[NH2:1][C:2]1[C:7]([Br:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.Br[CH2:11][C:12]([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1)=O.C(=O)([O-])O.[Na+]>C(O)C>[Br:8][C:7]1[C:2]2[N:3]([CH:11]=[C:12]([C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=3)[N:1]=2)[CH:4]=[C:5]([Cl:9])[CH:6]=1参加物
5
実験手順
17 g (82 mmol) of 2-amino-3-bromo-5-chloropyridine dissolved in 150 ml of ethanol are reacted with 29 g of 2-bromo-1-(4-chlorophenyl)-1-ethanone and 14 g of sodium hydrogen carbonate. The mixture is brought to the refluxing temperature for 6 h and cooled. The precipitate is filtered off and rinsed with CH2Cl2, and the filtrate is concentrated under reduced pressure. After recrystallization of the evaporation residue in ethyl acetate, the compound melts at 178° C.
後処理
- temperaturecooled
- filtrationThe precipitate is filtered off
- washrinsed with CH2Cl2
- concentrationthe filtrate is concentrated under reduced pressure
- customAfter recrystallization of the evaporation residue in ethyl acetate
出典と根拠
- ORDレコード
- ord-8a2f27f02afd4b7b85817dfa22b20cfb
- 出典データセット
- uspto-grants-1989_07
- 特許番号
- US04847263
関連ノート
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