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N,N-Dimethylaniline → 3-Chloro-6-(3-methyl-5-chloro-1-pyrazolyl)-pyridazine

HRID 27894
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반응식

HRID 27894 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([N:8]2[C:12](O)=[CH:11][C:10]([CH3:14])=[N:9]2)=[CH:6][CH:7]=1.P(Cl)(Cl)([Cl:17])=O.CN(C)C1C=CC=CC=1>>[Cl:1][C:2]1[N:3]=[N:4][C:5]([N:8]2[C:12]([Cl:17])=[CH:11][C:10]([CH3:14])=[N:9]2)=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 949N,N-DimethylanilineHCID 24813Phosphorus oxychlorideHCID 178429261HCID 178429261, 화합물

생성물 1

HCID 125628303-Chloro-6-(3-methyl-5-chloro-1-pyrazolyl)-pyridazine

반응 조건

온도
0 °C

실험 절차

To the mixture of 12.6 /0.04 moles/ of 3-chloro-6-(3-methyl-5-hydroxy-1-pyrazolyl)-pyridazine and 48 ml of phosphorus oxychloride, 7.28 g /0.04 moles/ of dimethyl aniline are dropped under stirring at 0° C. during half an hour, then the reaction mixture is stirred at room temperature for one hour and at boiling temperature for 2 hours. Excess of the phosphorus oxychloride is evaporated under reduced pressure, then the residue is poured into water and set aside overnight. The separated precipitate is filtered, washed with water and dried. Yield: 10.5 g (93%); m.p.: 123°-126° C.

후처리

  1. additionare dropped
  2. stirringthe reaction mixture is stirred at room temperature for one hour
  3. customfor 2 hours
  4. customExcess of the phosphorus oxychloride is evaporated under reduced pressure
  5. additionthe residue is poured into water
  6. filtrationThe separated precipitate is filtered
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-eef4ce6b3b1249df9a4b9ff555de8d47
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04224325

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