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Hydrochloric Acid → 1-(16-Oxoheptadecyl)-3,7-dimethylxanthine

HRID 964555
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 964555
C(Cl)(=O)C(Cl)=O.CS(C)=O.[OH:11][CH:12]([CH3:41])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][N:28]1[C:37](=[O:38])[C:36]2[N:35]([CH3:39])[CH:34]=[N:33][C:32]=2[N:31]([CH3:40])[C:29]1=[O:30].C(N(CC)CC)C.Cl>ClCCl>[O:11]=[C:12]([CH3:41])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][N:28]1[C:37](=[O:38])[C:36]2[N:35]([CH3:39])[CH:34]=[N:33][C:32]=2[N:31]([CH3:40])[C:29]1=[O:30]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 313Hydrochloric AcidHCID 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 232958871-(16-Hydroxyheptadecyl)-3,7-dimethylxanthine

Produkt 1

HCID 190774341-(16-Oxoheptadecyl)-3,7-dimethylxanthineAusbeute 47 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

To a solution of oxalyl chloride (0.036 ml, 0.41 mmol) in dichloromethane (3 ml) at -78° C. was added dimethylsulfoxide (0.063 ml, 0.82 mmol), and over 5 minutes, 1-(16-hydroxyheptadecyl)-3,7-dimethylxanthine (0.15 g, 0.35 mmol) in dichlorornethane (2 ml). The resulting reaction mixture was stirred at -78° C. for 30 minutes, and after the addition of triethylamine (0.23 ml, 1.64 mmol), was allowed to warm to 25° C. olier 30 minutes. Hydrochloric acid (1.0M, 10 ml) and dichloromethane (5 ml) were added to the warmed reaction mixture. The organic phase was separated and the aqueous phase was washed with dichlorornethane (10 ml). The organic portions were combined, dried over magnesium sulfate and evaporated to obtain a slightly yellow solid. The yellow solid, purified by chromatography (silica, ethyl acetate/hexane) resulted in 0.070 g of 1-(16-oxoheptadecyl)-3,7-dimethylxanthine as a white solid (47% yield).

Aufarbeitung

  1. customThe resulting reaction mixture
  2. temperatureto warm to 25° C. olier 30 minutes
  3. customThe organic phase was separated
  4. washthe aqueous phase was washed with dichlorornethane (10 ml)
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customto obtain a slightly yellow solid
  8. customThe yellow solid, purified by chromatography (silica, ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-2a31c0e748814af1aba98d9ecd346195
Quelldatensatz
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05770595

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