Nitric Acid → 2,3-dichloro-6-nitrobenzaldehyde

HRID 41353

反応式

HRID 41353 の反応式
[Cl:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([N+:11]([O-:13])=[O:12])[C:3]=1[CH:4]=[O:5]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 357452,3-Dichlorobenzaldehyde

生成物 1

HCID 112182712,3-dichloro-6-nitrobenzaldehyde

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

To 2,3-dichlorobenzaldehyde (20 g, 114 mmol) in concentrated sulfuric acid (100 mL) was added cautiously fuming nitric acid (5.4 mL, 8.16 g, 130 mmol). The resulting solution was stirred for 1 hour, then poured onto an ice/water slurry and the precipitate collected by filtration. This was dissolved in diethyl ether (400 mL), and the solution washed with water and saturated sodium carbonate, then dried (MgSO4) and concentrated. The residue was re-dissolved in the minimum amount of hot diethyl ether, then poured quickly into vigorously stirred petrol (1 L). After stirring for a further 10 minutes, the precipitate was collected by suction filtration and dried under vacuum to yield 2,3-dichloro-6-nitrobenzaldehyde, 9.98 g (40%), essentially free of isomers.

後処理

  1. filtrationthe precipitate collected by filtration
  2. dissolutionThis was dissolved in diethyl ether (400 mL)
  3. washthe solution washed with water and saturated sodium carbonate
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. dissolutionThe residue was re-dissolved in the minimum amount of hot diethyl ether
  7. additionpoured quickly into vigorously stirred petrol (1 L)
  8. stirringAfter stirring for a further 10 minutes
  9. filtrationthe precipitate was collected by suction filtration
  10. customdried under vacuum

出典と根拠

ORDレコード
ord-4d805f135fb64ccb8ca0b8cf87bb4f3f
出典データセット
uspto-grants-2013_09
特許番号
US08530651B2

関連ノート

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