Ammonia → 2,6-Dimethyl-5-nitroquinoline

HRID 2055013

反応式

HRID 2055013 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH3:12])[CH:8]=2)[N:3]=1.S(=O)(=O)(O)O.[N+:18]([O-])([O-:20])=[O:19].[K+].N>>[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH3:12])[C:8]=2[N+:18]([O-:20])=[O:19])[N:3]=1

参加物

5

反応物 4

HCID 222AmmoniaHCID 1118Sulfuric Acid2 回HCID 134142,6-DimethylquinolineHCID 24434Potassium Nitrate

生成物 1

HCID 7665652,6-Dimethyl-5-nitroquinoline

実験手順

3 g (19.08 mmol) of 2,6-dimethylquinoline is introduced into 15 ml of concentrated sulfuric acid at 10° C. After one-half hour, a solution of 2.03 g of potassium nitrate in 11.4 concentrated sulfuric acid is added in drops, specifically so that the temperature remains between 5° and 15° C. The batch is stirred for one more hour and then poured onto ice water. It is made ammonia-alkaline, and the deposited precipitate is suctioned off. After washing with water, the crude product is dissolved in ethyl acetate and shaken from water. The organic phase is treated as usual. After the solvent is spun off, 3.69 g (95.6%) of the desired compound remains, which is used in the reduction without further purification.

後処理

  1. waitAfter one-half hour
  2. customremains between 5° and 15° C
  3. additionpoured onto ice water
  4. washAfter washing with water
  5. dissolutionthe crude product is dissolved in ethyl acetate
  6. stirringshaken from water
  7. additionThe organic phase is treated as usual
  8. customwhich is used in the reduction without further purification

出典と根拠

ORDレコード
ord-103e8b31a27a41449459f811fc7c2ee5
出典データセット
uspto-grants-2008_02
特許番号
US07329753B2

関連ノート

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