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

HRID 508485
ノート
印刷プレビュー

反応式

HRID 508485 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-01b523e218064f4190a387d10ef1dbc2
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096525B2

反応ノート

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