Sodium Carbonate → {8-Fluoro-1,4-dioxaspiro[4.5]decan-8-yl}methanol

HRID 573212Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 573212
[FH:1].N1C=CC=CC=1.O1[C:10]2([CH2:19][CH2:18][CH2:17][CH2:16][C:13]3([O:15][CH2:14]3)[O:12][CH2:11]2)C1.[C:20]([O-:23])([O-])=O.[Na+].[Na+]>ClCCl>[F:1][C:18]1([CH2:20][OH:23])[CH2:17][CH2:16][C:13]2([O:12][CH2:11][CH2:14][O:15]2)[CH2:10][CH2:19]1

Komponenten

6

Edukt 4

HCID 10340Sodium CarbonateHCID 64774Pyridine, hydrofluoride (1:1)HCID 86647914HCID 86647914, VerbindungHCID 178435160HCID 178435160, Verbindung

Produkt 1

HCID 67225989{8-Fluoro-1,4-dioxaspiro[4.5]decan-8-yl}methanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of pyridine hydrofluoride (4 g) in dichloromethane (10 mL) was added dropwise to a solution of EXAMPLE 443A (1.7 g) in dichloromethane (20 mL) in a polyethylene bottle at 0° C. The mixture was stirred at room temperature overnight. The mixture was carefully poured over a mixture of ice-water and Na2CO3 and extracted with ethyl acetate (2×300 mL). After washing with water and brine, the organic layer was dried over Na2SO4, and filtered. Concentration of the filtrate gave the crude product.

Aufarbeitung

  1. extractionextracted with ethyl acetate (2×300 mL)
  2. washAfter washing with water and brine
  3. dry with materialthe organic layer was dried over Na2SO4
  4. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-be6fec7e800449769b81bcf00e38a8c0
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09029404B2

Notizen zur Reaktion

Wird geladen…