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

HRID 839228

반응식

HRID 839228 반응식
[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]

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

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].

후처리

  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

출처 및 근거

ORD 기록
ord-5d8967682a2c4ddfacb5de96cc45fbc9
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093812

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