Phosphorus oxychloride → 3-Chloro-6-(pyridin-2-yl)pyridazine

HRID 574181

反応式

HRID 574181 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[CH:8]=[CH:9][C:10](=O)[NH:11][N:12]=1.C([O-])(O)=O.[Na+].P(Cl)(Cl)([Cl:21])=O>>[Cl:21][C:10]1[N:11]=[N:12][C:7]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)=[CH:8][CH:9]=1

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 49800226-(Pyridin-2-yl)pyridazin-3-ol

生成物 1

HCID 64179603-Chloro-6-(pyridin-2-yl)pyridazine収率 95%

実験手順

4 g of pyridinylpyridazinone 7 dissolved in an excess (40 ml) of phosphorus oxychloride are refluxed for 8 hours. After cooling, the reaction mixture is poured into 250 ml of ice-cold water and then neutralized, dropwise, with a saturated aqueous solution of NaHCO3. After extraction with dichloromethane (5×100 ml), the organic phase is dried over MgSO4 and then concentrated under reduced pressure, to give the chlorinated pyridazine 8a with a yield of 95%.

後処理

  1. temperatureare refluxed for 8 hours
  2. temperatureAfter cooling
  3. extractionAfter extraction with dichloromethane (5×100 ml)
  4. dry with materialthe organic phase is dried over MgSO4
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1936cf7539f34b22b52f3709464007ec
出典データセット
uspto-grants-2015_05
特許番号
US09034873B2

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