Triethylamine → HCID 13715102, Verbindung

HRID 703556Notizen

Reaktionsgleichung

[Cl:1][C:2]1[CH:28]=[CH:27][C:5]([CH2:6][O:7][C@@H:8]2[C@@H:12]([CH2:13][O:14][C:15](=[O:17])[CH3:16])[O:11][C@@H:10]([N:18]3[CH:25]=[C:24]([F:26])[C:22](=[O:23])[NH:21][C:19]3=[O:20])[CH2:9]2)=[CH:4][CH:3]=1.[CH2:29]([O:32][C:33]1[CH:41]=[CH:40][C:36]([C:37](Cl)=[O:38])=[CH:35][CH:34]=1)[CH2:30][CH3:31].C(N(CC)CC)C>O1CCOCC1>[C:15]([O:14][CH2:13][C@H:12]1[O:11][C@@H:10]([N:18]2[CH:25]=[C:24]([F:26])[C:22](=[O:23])[N:21]([C:37](=[O:38])[C:36]3[CH:35]=[CH:34][C:33]([O:32][CH2:29][CH2:30][CH3:31])=[CH:41][CH:40]=3)[C:19]2=[O:20])[CH2:9][C@@H:8]1[O:7][CH2:6][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:28][CH:27]=1)(=[O:17])[CH3:16]

Komponenten

Reaktionsbedingungen

Temperatur: 70 °C

Versuchsvorschrift

To a solution of 0.30 g of 3'-O-(4-chlorobenzyl)-5'-O-acetyl-2'-deoxy-5-fluorouridine in 30 ml of dioxane were added 0.44 g of 4-n-propoxybenzoyl chloride and 0.61 ml of triethylamine, and the mixture was stirred at 70° C. for 3 hours. The insolubles were removed by filtration, and the residue was dissolved in ethyl acetate. The solution was washed with water and dried. The ethyl acetate was distilled off, and the residue was placed on a silica gel column and eluted with chloroform-petroleum ether (1:1), thereby producing 0.15 g of the title compound in a yield of 36%.

Aufarbeitung

customThe insolubles were removed by filtration
dissolutionthe residue was dissolved in ethyl acetate
washThe solution was washed with water
customdried
distillationThe ethyl acetate was distilled off
washeluted with chloroform-petroleum ether (1:1)

Quellen und Nachweise

ORD-Eintrag: ord-2a1fecf3abad49399f3f365c4340d53a
Quelldatensatz: uspto-grants-1991_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04983609

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