Phosphorus oxychloride → 3-(5-Nitrofuran-2-yl)-1-phenyl-1H-pyrazole-4-carboxamide

HRID 839228

反応式

HRID 839228 の反応式
[N+:1]([C:4]1[O:8][C:7]([C:9]2[C:13]([C:14](O)=[O:15])=[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.[N+:28](C1OC(C2C(C(Cl)=O)=CN(C3C=CC=CC=3)N=2)=CC=1)([O-])=O>ClC(Cl)C>[N+:1]([C:4]1[O:8][C:7]([C:9]2[C:13]([C:14]([NH2:28])=[O:15])=[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]

参加物

5

反応物 3

HCID 24813Phosphorus oxychlorideHCID 203259333-(5-Nitrofuran-2-yl)-1-phenyl-1H-pyrazole-4-carbonyl chlorideHCID 203259643-(5-Nitrofuran-2-yl)-1-phenyl-1H-pyrazole-4-carboxylic acid

生成物 1

HCID 203261233-(5-Nitrofuran-2-yl)-1-phenyl-1H-pyrazole-4-carboxamide

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

Heat 1 g of 3-(5-nitro-2-furyl)-1-phenylpyrazole-4-carboxylic acid together with 0.56 g of phosphorus oxychloride and 10 ml of dichloroethane for 2 hours at 80° C. Add 10 ml of a 25% aqueous solution dropwise at 0° C to the thus-obtained solution of 3-(5-nitro-2-furyl)-1-phenylpyrazole-4-carboxylic chloride. Allow the resulting mixture to stand overnight and then vacuum distil it to remove the organic solvent therefrom. Vacuum filter to separate formed precipitate and recrystallize the filter residue from dimethylformamide/methanol to obtain 3-(5-nitro-2-furyl)-1-phenylpyrazole-4-carboxamide [m.p. 236° to 238° C].

後処理

  1. customvacuum distil it
  2. customto remove the organic solvent
  3. filtrationVacuum filter
  4. customto separate
  5. customformed precipitate
  6. customrecrystallize the filter residue from dimethylformamide/methanol

出典と根拠

ORDレコード
ord-5d8967682a2c4ddfacb5de96cc45fbc9
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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