Sodium Hydroxide → HCID 23359208, Verbindung

HRID 232870Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 232870
[OH-].[Na+].[C:3]([C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11]C)=[O:10])=[C:7]([CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)[CH:6]=1)#[N:4]>CO>[C:3]([C:5]1[CH:14]=[CH:13][C:8]([C:9]([OH:11])=[O:10])=[C:7]([CH2:15][O:16][C:17]2[CH:18]=[CH:19][C:20]([OH:23])=[CH:21][CH:22]=2)[CH:6]=1)#[N:4]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 23359186Methyl 4-cyano-2-[(4-hydroxyphenoxy)methyl]benzoate

Produkt 1

HCID 23359208HCID 23359208, VerbindungAusbeute 57,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

20 ml of a 3N-sodium hydroxide aqueous solution was added to 9.5 g of methyl 4-cyano-2-(4-hydroxyphenoxy)methylbenzoate obtained in Reference example 22 dissolved in 80 ml of methanol and the mixture was stirred at room temperature for 1.5 hours. After completion of the reaction, the solvent was removed under reduced pressure, water was added to the residue and the mixture was washed with diethyl ether and then adjusted to about pH 2 with conc. sulfuric acid. Crystals precipitated were collected by filtration and dissolved in ethyl acetate and the organic layer was washed with a saturated saline solution and then dried over anhydrous sodium sulfate. The solvent was removed from the solution to obtain 5.2 g of the title compound.

Aufarbeitung

  1. customobtained in Reference example 22
  2. customAfter completion of the reaction
  3. customthe solvent was removed under reduced pressure, water
  4. additionwas added to the residue
  5. washthe mixture was washed with diethyl ether
  6. customCrystals precipitated
  7. filtrationwere collected by filtration
  8. dissolutiondissolved in ethyl acetate
  9. washthe organic layer was washed with a saturated saline solution
  10. dry with materialdried over anhydrous sodium sulfate
  11. customThe solvent was removed from the solution

Quellen und Nachweise

ORD-Eintrag
ord-b51d0f5ed7534c8aadb14df8ff17d738
Quelldatensatz
uspto-grants-1997_01
Patentnummer
US05591752

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