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Quinoline → 3-Bromo-2-chloro-4-methyl-5-nitropyridine

HRID 508485
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HRID 508485 반응식
[Cl-:1].[P+]=O.N1C2C(=CC=CC=2)C=CC=1.[Br:14][C:15]1[C:16](=O)[NH:17][CH:18]=[C:19]([N+:22]([O-:24])=[O:23])[C:20]=1[CH3:21]>O>[Br:14][C:15]1[C:16]([Cl:1])=[N:17][CH:18]=[C:19]([N+:22]([O-:24])=[O:23])[C:20]=1[CH3:21]
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참가 물질

5

반응물 3

HCID 7047QuinolineHCID 401519143-Bromo-4-methyl-5-nitro-1,2-dihydropyridin-2-oneHCID 178527006HCID 178527006, 화합물

생성물 1

HCID 401519173-Bromo-2-chloro-4-methyl-5-nitropyridine

시약·촉매·용매 1

HCID 962Water용매

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온도
120 °C

실험 절차

In a 25 ml single-necked round-bottomed flask, to 1.72 ml phosphorous oxide chloride kept at a temperature of 5° C., 0.857 ml quinoline and 3.40 g of 3-bromo-4-methyl-5-nitro-1H-pyridin-2-one are added consecutively. The resulting beige suspension is stirred under heating to 120° C. whereupon a brown solution is obtained. Stirring is continued for 2 hours. Afterwards, the solution is cooled down to an ambient temperature and poured into water. The resulting precipitate is collected by filtration, the filter cake washed with water (4×) and dried to give 3.15 g of the title compound in the form of a brown solid (MP: 60-62° C.).

후처리

  1. additionare added consecutively
  2. customis obtained
  3. stirringStirring
  4. temperatureAfterwards, the solution is cooled down to an ambient temperature
  5. filtrationThe resulting precipitate is collected by filtration
  6. washthe filter cake washed with water (4×)
  7. customdried

출처 및 근거

ORD 기록
ord-01b523e218064f4190a387d10ef1dbc2
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096525B2

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