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Pyridine → 3,5-didecoxybenzyl Chloride

HRID 2055753
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2055753
CN(C=O)C.S(Cl)([Cl:8])=O.[CH2:10]([O:20][C:21]1[CH:22]=[C:23]([CH:26]=[C:27]([O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])[CH:28]=1)[CH2:24]O)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].N1C=CC=CC=1>ClCCl>[CH2:10]([O:20][C:21]1[CH:22]=[C:23]([CH:26]=[C:27]([O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39])[CH:28]=1)[CH2:24][Cl:8])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 1049PyridineHCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 577763673,5-Didecyloxybenzyl Alcohol

Produkt 1

HCID 693060093,5-didecoxybenzyl ChlorideAusbeute 94,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344
Dichloromethane
Lösungsmittel
3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Dry dichloromethane (5 mL), DMF (3.04 mL, 39.2 mmol), and a magnetic stir bar were placed into a 250 mL RBF and sealed with a rubber septum. N2 inlet and outlet needles were inserted into the septum. The flask was then cooled to 0° C. in an ice bath. Thionyl chloride (2.86 mL, 39.2 mmol) was added to the RBF via a syringe. The RBF was placed into an ice bath and cooled to 0° C. 3,5-didecoxybenzyl alcohol (15.0 g, 35.7 mmol) was dissolved in a solution of dichloromethane (60 mL) containing pyridine (2.88 mL, 35.7 mmol). This solution was then drawn into a syringe and added cautiously to RBF over 20 minutes. The solution gradually changed from a transparent yellow color to an opaque yellow color. Dichloromethane was used to rinse the beaker which was used to dissolve 3,5-didecoxybenzyl alcohol and then added to the RBF. The RBF was removed from the ice bath and allowed to stir overnight. The solution was then concentrated using a rotary evaporation. A solution of 50/50 ether/hexanes (100 mL) was added to the RBF, changing the solution from deep yellow to opaque white. The liquid was decanted off leaving behind any solid. The RBF was rinsed in this manner 2 more times, saving the decanted liquid. The decanted liquid was run through a silica gel baseline filtration apparatus. Filtrate was then concentrated using rotary evaporation. A compound solidified after approximately 2 hours under a high vacuum. There was a 14.8 g yield or a 94.5% yield of the derivative. The NMR characterization data for this derivative is as follows. 1NMR (300 MHz, CDCl3): 0.88 (t, J=6.6, 6H, CH2CH3), 1.27-1.43 (m, 28H, CH2(CH2)7), 1.76 (p, J=6.6, 4H, OCH2CH2), 3.92 (t, J=6.6, 4H, OCH2), 4.50 (s, 2H, ArCH2Cl), 6.39 (t, J=2.2, 1H, ArH), 6.50 (d, J=2.5, 2H, ArH). 13C NMR (75 MHZ, CDCl3): 14.23, 22.78, 26.12, 29.30, 29.42, 29.47, 29.70, 32.00, 46.56, 68.18, 101.332, 106.97, 139.38, 160.52.

Aufarbeitung

  1. customsealed with a rubber septum
  2. customN2 inlet and outlet needles were inserted into the septum
  3. customThe RBF was placed into an ice bath
  4. temperaturecooled to 0° C
  5. customThis solution was then drawn into a syringe
  6. additionadded cautiously
  7. washto rinse the beaker which
  8. dissolutionto dissolve 3,5-didecoxybenzyl alcohol
  9. additionadded to the RBF
  10. customThe RBF was removed from the ice bath
  11. concentrationThe solution was then concentrated
  12. customa rotary evaporation
  13. additionA solution of 50/50 ether/hexanes (100 mL) was added to the RBF
  14. customThe liquid was decanted off
  15. customleaving behind any solid
  16. washThe RBF was rinsed in this manner 2 more times
  17. filtrationThe decanted liquid was run through a silica gel baseline filtration apparatus
  18. concentrationFiltrate was then concentrated
  19. customevaporation
  20. waitA compound solidified after approximately 2 hours under a high vacuum
  21. customyield

Quellen und Nachweise

ORD-Eintrag
ord-54324171d6d7436495fa29a03f23ba05
Quelldatensatz
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07332529B2

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