反応式
[N+:1]([C:4]1[O:8][C:7]([C:9]2[C:13]([C:14]([NH2:16])=O)=[CH:12][N:11]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[N:10]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2].P(Cl)(Cl)(Cl)=O.[OH-].[Na+]>ClCCCl>[N+:1]([C:4]1[O:8][C:7]([C:9]2[C:13]([C:14]#[N:16])=[CH:12][N:11]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:10]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2]参加物
5
実験手順
Heat at its boiling point a mixture of 10 g of 3-(5-nitro-2-furyl)-1-phenylpyrazole-4-carboxamide and 16.5 g of phosphorus oxychloride in 100 ml of 1,2-dichloroethane for 1 hour. Pour the resulting solution onto ice, and adjust the pH-value to 4 with saturated caustic soda solution. Separate the organic phase. Wash it with water and then evaporate it to dryness to obtain a 95% yield of 3-(5-nitro-2-furyl)-1-phenylpyrazole-4-carbonitrile [m.p. 190° to 192° C].
後処理
- temperatureHeat at its boiling point
- additionPour the resulting solution onto ice
- customSeparate the organic phase
- washWash it with water
- customevaporate it to dryness
出典と根拠
- ORDレコード
- ord-02ce5c141d9f4185b794e6b791a8bd7b
- 出典データセット
- uspto-grants-1978_06
- 特許番号
- US04093812
関連ノート
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