Salicylic Acid → HCID 68880764, Verbindung

HRID 1166193

Reaktionsgleichung

Reaktionsgleichung von HRID 1166193
[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].Cl[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH2:19][Cl:20])[N:14]=1.[CH2:21]([O:23]CC)[CH3:22]>CN(C=O)C>[Cl:20][CH2:19][C:15]1[N:14]=[C:13]([CH3:12])[C:18]([O:9][C:1](=[O:10])[C:2]2[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=2[O:4][C:21](=[O:23])[CH3:22])=[CH:17][CH:16]=1

Komponenten

5

Edukt 3

HCID 338Salicylic AcidHCID 3283Diethyl EtherHCID 3166542,6-Bis(chloromethyl)pyridine

Produkt 1

HCID 68880764HCID 68880764, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

To a solution of salicylic acid (1.6 g, 8.88 mmoles) in N,N′-dimethylformamide (20 ml) and under stirring sodium ethylate (0.64 g, 8.88 mmoles) is added. After 30 minutes the obtained solution is added to a solution of 2,6-bis-(chloromethyl)pyridine (4.72 g, 26.81 mmoles) in N,N′-dimethylformamide (20 ml). The solution is left at room temperature for 7 days, under stirring, then is diluted with ethyl ether and washed with water. The separated organic phases are anhydrified with sodium sulphate and the solvent is evaporated at reduced pressure. The reaction crude product is purified by chromatography on silica gel by eluting with n-hexane/ethyl acetate 7/3. 1.7 g of the product as yellow oil are obtained.

Aufarbeitung

  1. washwashed with water
  2. customthe solvent is evaporated at reduced pressure
  3. customThe reaction crude product
  4. customis purified by chromatography on silica gel
  5. washby eluting with n-hexane/ethyl acetate 7/3

Quellen und Nachweise

ORD-Eintrag
ord-b05a90314d204242a2ac14f8fc776bbd
Quelldatensatz
uspto-grants-2003_09
Patentnummer
US06613784B1

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