HCID 178493296, Verbindung → 2-(2-Diisopropylaminoethylamino)-4-methoxypyridine

HRID 1395555Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1395555
[CH:1]([N:4]([CH:17]([CH3:19])[CH3:18])[CH2:5][CH2:6][NH:7][C:8]1[CH:13]=[C:12]([O:14][CH3:15])[CH:11]=[CH:10][N+:9]=1[O-])([CH3:3])[CH3:2]>C(O)(=O)C.[Fe]>[CH:17]([N:4]([CH:1]([CH3:3])[CH3:2])[CH2:5][CH2:6][NH:7][C:8]1[CH:13]=[C:12]([O:14][CH3:15])[CH:11]=[CH:10][N:9]=1)([CH3:18])[CH3:19]

Komponenten

4

Edukt 1

HCID 178493296HCID 178493296, Verbindung

Produkt 1

HCID 128576332-(2-Diisopropylaminoethylamino)-4-methoxypyridine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

2-(2-diisopropylaminoethylamino)-4-methoxypyridine-N-oxide (4.3 g., 15 mmole) dissolved in glacial acetic acid (32 ml.) is refluxed with iron powder (8.2 g.) for three hours. The reaction mixture is filtered to remove insoluble salts and then the solvent evaporated. The residue is dissolved in methanol, treated with excess potassium hydroxide pellets and filtered to remove more insoluble salts. The concentrate solution is dissolved in chloroform, washed with water, dried over sodium sulfate, filtered through a pad of charcoal and evaporated to give oily product.

Aufarbeitung

  1. filtrationThe reaction mixture is filtered
  2. customto remove insoluble salts
  3. customthe solvent evaporated
  4. dissolutionThe residue is dissolved in methanol
  5. additiontreated with excess potassium hydroxide pellets
  6. filtrationfiltered
  7. customto remove more insoluble salts
  8. dissolutionThe concentrate solution is dissolved in chloroform
  9. washwashed with water
  10. dry with materialdried over sodium sulfate
  11. filtrationfiltered through a pad of charcoal
  12. customevaporated
  13. customto give oily product

Quellen und Nachweise

ORD-Eintrag
ord-41f86ab7b419465b93bad7cb1b735ee9
Quelldatensatz
uspto-grants-1980_05
Patentnummer
US04203988

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