StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Diethyl Ether → HCID 131722977, Verbindung

HRID 428818
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 428818
[OH:1][C:2]([CH3:23])([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:3]/[CH:4]=[CH:5]/[Sn](CCCC)(CCCC)CCCC.C(OCC)C.C[Li].[Cu]C#N.[Si:34]([O:41][CH:42]1[CH2:46][C:45](=[O:47])[C:44]([CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][C:54]([O:56][CH3:57])=[O:55])=[CH:43]1)([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35].[Cl-].[NH4+]>O1CCCC1>[CH3:57][O:56][C:54](=[O:55])[CH2:53][CH2:52][CH2:51][CH2:50][CH2:49][CH2:48][C@@H:44]1[C@@H:43](/[CH:5]=[CH:4]/[CH2:3][C:2]([OH:1])([CH3:23])[CH2:19][CH2:20][CH2:21][CH3:22])[CH:42]([O:41][Si:34]([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:35])[CH3:36])[CH2:46][C:45]1=[O:47]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 3283Diethyl EtherHCID 25517Ammonium ChlorideHCID 4653916Methyl 7-(3-((tert-butyldimethylsilyl)oxy)-5-oxocyclopent-1-en-1-yl)heptanoateHCID 11026395HCID 11026395, VerbindungHCID 178418348HCID 178418348, VerbindungHCID 178418546HCID 178418546, Verbindung

Produkt 1

HCID 131722977HCID 131722977, VerbindungAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
-40 °C

Versuchsvorschrift

Into a dry flask was placed a solution of [(4RS, 1E)-4-hydroxy-4-methyl-1-octenyl]tri-n-butyltin (1.36 g, 3.15 mmol) in dry tetrahydrofuran (5 ml) under nitrogen atmosphere, and the mixture was cooled to 0° C. To this solution was dropped 5.7 ml (5.99 mmol) of a diethyl ether solution of methyllithium (1.05 mol/liter), and stirring was continued for 1 h, letting the temperature rise gradually to room temperature. After cooling to −40° C., copper (I) cyanide (141 mg, 1.58 mmol) was added and dissolved by letting the temperature rise gradually to 0° C. This reaction liquid was cooled to −78° C. and added with a solution of (±) methyl 7-(3-tert-butyldimethylsilyloxy-5-oxo-1-cyclopentenyl)heptanoate (318 mg, 0.9 mmol) in dry tetrahydrofuran (1.5 ml) was rapidly added. After stirring for 5 min, 20 ml of a saturated aqueous ammonium chloride/aqueous ammonia (9:1) was added, and stirring was continued for 30 min , letting the temperature rise gradually to room temperature. This mixture was extracted with ethyl acetate (80 ml) two times, and the combined organic layer was washed with a saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and concentrated in vacuo to remove solvent. The residue was purified by silica gel column chromatography [ethyl acetate/hexane (1/5)] to give 413 mg (96% yield) of (±)-methyl(16RS, 13E)-11-tert-butyldimethylsilyloxy-16-hydroxy-16-methyl-9-oxoprost-13-en-1-oate as a colorless oil. The spectral data of IR and 1H NMR were identical with those of the example 2.

Aufarbeitung

  1. customInto a dry flask was placed
  2. customgradually to room temperature
  3. dissolutiondissolved
  4. customgradually to 0° C
  5. customThis reaction liquid
  6. temperaturewas cooled to −78° C.
  7. additionwas rapidly added
  8. stirringAfter stirring for 5 min
  9. stirringstirring
  10. waitwas continued for 30 min
  11. customgradually to room temperature
  12. extractionThis mixture was extracted with ethyl acetate (80 ml) two times
  13. washthe combined organic layer was washed with a saturated aqueous sodium chloride
  14. dry with materialdried over anhydrous magnesium sulfate
  15. concentrationconcentrated in vacuo
  16. customto remove solvent
  17. customThe residue was purified by silica gel column chromatography [ethyl acetate/hexane (1/5)]

Quellen und Nachweise

ORD-Eintrag
ord-f0c1f8103e414a6897080845d32f0525
Quelldatensatz
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06313341B1

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion