Potassium Hydroxide → 5-(1-Adamantylethynyl)isophthalic acid dipotassium salt

HRID 1994660

Reaktionsgleichung

Reaktionsgleichung von HRID 1994660
[OH-].[K+:2].C[O:4][C:5]([C:7]1[CH:8]=[C:9]([C:17]#[C:18][C:19]23[CH2:28][CH:23]4[CH2:24][CH:25]([CH2:27][CH:21]([CH2:22]4)[CH2:20]2)[CH2:26]3)[CH:10]=[C:11]([C:13]([O:15]C)=[O:14])[CH:12]=1)=[O:6]>C(O)CCC>[K+:2].[K+:2].[C:19]12([C:18]#[C:17][C:9]3[CH:10]=[C:11]([C:13]([O-:15])=[O:14])[CH:12]=[C:7]([CH:8]=3)[C:5]([O-:6])=[O:4])[CH2:20][CH:21]3[CH2:22][CH:23]([CH2:24][CH:25]([CH2:27]3)[CH2:26]1)[CH2:28]2

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 675073001-(3,5-Bis(methoxycarbonyl)phenyl)-2-(1-adamantyl)ethyne

Produkt 1

HCID 675066175-(1-Adamantylethynyl)isophthalic acid dipotassium saltAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

In a 5 L four-neck flask provided with a thermometer, a Dimroth condenser and an agitator, 3 L of n-butanol and 226 g of potassium hydroxide (85%) (2.72 mol) were charged. The mixture was heated and refluxed to be dissolved. After adding 120 g of the obtained 1-(3,5-bis(methoxycarbonyl)phenyl)-2-(1-adamantyl)ethyne (0.341 mol) therein, the mixture was heated and refluxed for 30 minutes. Next, it was cooled in an ice bath and filtered to obtain precipitated crystal. The crystal was washed with 1 L of ethanol two times followed by drying under pressure at 60° C., thus obtaining 132.49 g of 5-(2-(1-adamantyl)ethynyl) isophthalic acid dipotassium salt (the yield was 97%).

Aufarbeitung

  1. customIn a 5 L four-neck flask provided with a thermometer
  2. temperatureThe mixture was heated
  3. temperaturerefluxed
  4. dissolutionto be dissolved
  5. temperaturethe mixture was heated
  6. temperaturerefluxed for 30 minutes
  7. temperatureNext, it was cooled in an ice bath
  8. filtrationfiltered
  9. customto obtain
  10. customprecipitated crystal
  11. washThe crystal was washed with 1 L of ethanol two times
  12. customby drying under pressure at 60° C.

Quellen und Nachweise

ORD-Eintrag
ord-13a4d2f0e7544239ab7abc05a4ff91b6
Quelldatensatz
uspto-grants-2010_01
Patentnummer
US07652125B2

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