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Hydrogen Peroxide → 5-Decyloxy-2-{4-(6-hydroxy-1-trans-heptenyl)-phenyl}-pyrimidine

HRID 725675
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 725675
[CH2:1]([O:11][C:12]1[CH:13]=[N:14][C:15]([C:18]2[CH:23]=[CH:22][C:21](Br)=[CH:20][CH:19]=2)=[N:16][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[OH-].[Na+].[OH:27][CH:28]([CH3:37])[CH2:29][CH2:30][CH2:31]/[CH:32]=[CH:33]/B(O)O.OO>O1CCCC1.C(Cl)(Cl)Cl>[CH2:1]([O:11][C:12]1[CH:13]=[N:14][C:15]([C:18]2[CH:23]=[CH:22][C:21](/[CH:33]=[CH:32]/[CH2:31][CH2:30][CH2:29][CH:28]([OH:27])[CH3:37])=[CH:20][CH:19]=2)=[N:16][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 784Hydrogen PeroxideHCID 14798Sodium Hydroxide2×HCID 114747935-Decyloxy-2-(4-bromophenyl)pyrimidineHCID 19352669E-6-hydroxy-1-heptenyldihydroxyborane

Produkt 1

HCID 193525205-Decyloxy-2-{4-(6-hydroxy-1-trans-heptenyl)-phenyl}-pyrimidineAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Apart from the above, inner atmosphere of a four-necked flask equipped with a stirring device, a reflux condenser and a thermometer was replaced with nitrogen gas, and then the flask was charged with 6.6 g (17 mmol) of 5-decyloxy-2-(4-bromophenyl)-pyrimidine, 0.23 g (0.2 mmol) of tetrakis-triphenylphosphine-palladium, 2.4 g (60 mmol) of sodium hydroxide and 60 ml of tetrahydrofuran. Subsequently, 50 ml of a solution prepared by dissolving 20 mmol of the above-obtained E-6-hydroxy-1-heptenyldihydroxyborane in tetrahydrofuran was dropwise added thereto at room temperature. Then, the whole mixture was heated under reflux with stirring for 6 hours. After cooling the reaction mixture to room temperature, 5 ml of 10% aqueous solution of sodium hydroxide and 2 ml of 30% aqueous solution of hydrogen peroxide were added, and the resulting mixture was stirred for one hour. The mixture was extracted with ether, and the organic layer was twice washed with each 20 ml portion of saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography to obtain 5.9 g (yield 82%) of (-)-5-decyloxy-2-{4-(6-hydroxy-1-trans-heptenyl)-phenyl}-pyrimidine, [α]D20 =-1.2 (c=1.0, CHCl3).

Aufarbeitung

  1. customApart from the above, inner atmosphere of a four-necked flask equipped with a stirring device, a reflux condenser
  2. additionwas dropwise added
  3. customat room temperature
  4. temperatureThen, the whole mixture was heated
  5. temperatureunder reflux
  6. stirringthe resulting mixture was stirred for one hour
  7. extractionThe mixture was extracted with ether
  8. washthe organic layer was twice washed with each 20 ml portion of saturated aqueous solution of sodium chloride
  9. dry with materialdried over anhydrous magnesium sulfate
  10. distillationThe solvent was distilled off
  11. customthe residue was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-951de6a8ef564322b18ed73e079caa02
Quelldatensatz
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05707547

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