Ethanol → 3-(3-Dimethoxymethyl-4-nitrophenoxy)-benzonitrile

HRID 390272ノート

反応式

HRID 390272 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1)#[N:2].[C:10]([O-:13])([O-])=O.[K+].[K+].F[C:17]1[CH:18]=[CH:19][C:20]([N+:25]([O-:27])=[O:26])=[C:21]([CH:24]=1)[CH:22]=[O:23].[CH2:28](O)C>>[CH3:28][O:23][CH:22]([O:13][CH3:10])[C:21]1[CH:24]=[C:17]([CH:18]=[CH:19][C:20]=1[N+:25]([O-:27])=[O:26])[O:9][C:5]1[CH:4]=[C:3]([CH:8]=[CH:7][CH:6]=1)[C:1]#[N:2]

参加物

5

反応物 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 133943-CyanophenolHCID 5870905-Fluoro-2-nitrobenzaldehyde

生成物 1

HCID 586250533-(3-Dimethoxymethyl-4-nitrophenoxy)-benzonitrile

実験手順

A mixture of 3-cyanophenol (0.38 mol) in ethanol (600 mL) was stirred at room temperature and K2CO3 (0.29 mol) was added. 5-fluoro-2-nitrobenzaldehyde (0.18 mol) was added, and the reaction mixture was stirred and refluxed for 4 hours. The solvent was evaporated, and the residue was stirred in water and extracted with CH2Cl2. The organic layer was separated, dried, filtered off and the solvent was evaporated. The residue was triturated under diisopropyl ether, and then the formed solids were filtered off and dried to yield the title compound.

後処理

  1. stirringthe reaction mixture was stirred
  2. temperaturerefluxed for 4 hours
  3. customThe solvent was evaporated
  4. stirringthe residue was stirred in water
  5. extractionextracted with CH2Cl2
  6. customThe organic layer was separated
  7. customdried
  8. filtrationfiltered off
  9. customthe solvent was evaporated
  10. customThe residue was triturated under diisopropyl ether
  11. filtrationthe formed solids were filtered off
  12. customdried

出典と根拠

ORDレコード
ord-1f2124a3aa644c6faf7e1b14e328c3a7
出典データセット
uspto-grants-2013_02
特許番号
US08383637B2

反応ノート

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