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4-Chloro-2-nitroaniline → HCID 10846711, 화합물

HRID 1578690
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HRID 1578690 반응식
CO[CH:3]1[CH2:7][CH2:6][CH:5](OC)O1.[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[C:13]([N+:18]([O-:20])=[O:19])[CH:12]=1>C(O)(=O)C>[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([N:15]2[CH:3]=[CH:7][CH:6]=[CH:5]2)=[C:13]([N+:18]([O-:20])=[O:19])[CH:12]=1
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참가 물질

4

반응물 2

HCID 69794-Chloro-2-nitroanilineHCID 790982,5-Dimethoxytetrahydrofuran

생성물 1

HCID 10846711HCID 10846711, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

100 g (0.75 mole) of 2,5-dimethoxytetrahydrofuran are added dropwise to a stirred solution of 86.3 g (0.5 mole) of 4-chloro-2-nitroaniline in 500 ml. of glacial acetic acid. The solution is refluxed under a nitrogen atmosphere for 30 minutes, filtered, and poured into 2500 ml. of water. The aqueous solution is extracted with chloroform. The chloroform solution is dried with anhydrous sodium sulfate and concentrated to a brown oil. The brown oil is dissolved in an ether-petroleum ether-mixture and placed in a refrigerator overnight. An orange solid precipitates and is recrystallized from an ether petroleum ether mixture to give 1-(4-chloro-2-nitrophenyl) pyrrole, m.p. 55°-56° C.

후처리

  1. temperatureThe solution is refluxed under a nitrogen atmosphere for 30 minutes
  2. filtrationfiltered
  3. additionpoured into 2500 ml
  4. extractionThe aqueous solution is extracted with chloroform
  5. dry with materialThe chloroform solution is dried with anhydrous sodium sulfate
  6. concentrationconcentrated to a brown oil
  7. dissolutionThe brown oil is dissolved in an ether-petroleum ether-mixture
  8. customplaced in a refrigerator overnight
  9. customAn orange solid precipitates
  10. customis recrystallized from an ether petroleum ether mixture

출처 및 근거

ORD 기록
ord-491cab11651046f7aa76d2fcd23eeb2d
출처 데이터셋
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03939159

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