Water → 3-(5-nitro-2-furyl)-1H-pyrazole-4-carbonitrile

HRID 839218ノート

反応式

HRID 839218 の反応式
[N+:1]([C:4]1[O:8][C:7]([C:9]2[C:13]([CH:14]=[N:15]O)=[CH:12][NH:11][N:10]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2].P(Cl)(Cl)(Cl)=O.O.C(=O)([O-])O.[Na+]>ClCCCl>[N+:1]([C:4]1[O:8][C:7]([C:9]2[C:13]([C:14]#[N:15])=[CH:12][NH:11][N:10]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

6

反応物 4

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 178526569HCID 178526569、化合物

生成物 1

HCID 1785104403-(5-nitro-2-furyl)-1H-pyrazole-4-carbonitrile収率 96%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

Heat Then g. of 3-(5-nitro-2-furyl)-1H-pyrazole-4-carboxaldehydeoxime together with 3.4 g of phosphorus oxychloride in 20 ml of 1,2-dichloroethane for 1 hour under reflux. To the resulting product add ice together with 50 ml of water. The adjust the pH to from 3 to 4 with sodium hydrogen carbonate and remove the formed crystals by vacuum filtration. Wash the crystals with water to obtain a 96% yield of 3-(5-nitro-2-furyl)-1H-pyrazole-4-carbonitrile [m.p. 237.5° to 239° C (from ethanol)].

後処理

  1. temperatureHeat
  2. customremove the formed crystals
  3. filtrationby vacuum filtration
  4. washWash the crystals with water

出典と根拠

ORDレコード
ord-d0147a6b80da4f1aadf9c90ef54ae343
出典データセット
uspto-grants-1978_06
特許番号
US04093812

反応ノート

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