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

Ammonium Chloride → 1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17beta-{4-ethyl-4-(triethylsilyloxy)hexyloxymethyl}androst-5-ene

HRID 1792228
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1792228
[Si:1]([O:8][C@@H:9]1[C@@:26]2([CH3:27])[C:13](=[CH:14][CH2:15][C@@H:16]3[C@@H:25]2[CH2:24][CH2:23][C@@:21]2([CH3:22])[C@H:17]3[CH2:18][CH2:19][C@@H:20]2[CH2:28][OH:29])[CH2:12][C@@H:11]([O:30][Si:31]([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:33])[CH3:32])[CH2:10]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[H-].[K+].C1OCCOCCOCCOCCOCCOC1.Br[CH2:59][CH2:60][CH2:61][C:62]([CH2:73][CH3:74])([O:65][Si:66]([CH2:71][CH3:72])([CH2:69][CH3:70])[CH2:67][CH3:68])[CH2:63][CH3:64].[Cl-].[NH4+]>O1CCCC1>[Si:1]([O:8][C@@H:9]1[C@@:26]2([CH3:27])[C:13](=[CH:14][CH2:15][C@@H:16]3[C@@H:25]2[CH2:24][CH2:23][C@@:21]2([CH3:22])[C@H:17]3[CH2:18][CH2:19][C@@H:20]2[CH2:28][O:29][CH2:59][CH2:60][CH2:61][C:62]([CH2:73][CH3:74])([O:65][Si:66]([CH2:71][CH3:72])([CH2:67][CH3:68])[CH2:69][CH3:70])[CH2:63][CH3:64])[CH2:12][C@@H:11]([O:30][Si:31]([C:34]([CH3:37])([CH3:36])[CH3:35])([CH3:32])[CH3:33])[CH2:10]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 25517Ammonium ChlorideHCID 2855718-Crown-6HCID 82127Potassium hydrideHCID 220276701-Bromo-4-ethyl-4-(triethylsilyloxy)hexaneHCID 696299821alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17beta-(hydroxymethyl)androst-5-ene

Produkt 1

HCID 69630124
1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17beta-{4-ethyl-4-(triethylsilyloxy)hexyloxymethyl}androst-5-ene
Ausbeute 99,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

1α,3β-Bis(tert-butyldimethylsilyloxy)-17β-(hydroxymethyl)androst-5-ene (11.0 g) was dissolved in tetrahydrofuran. Under cooling with ice, potassium hydride (30% in oil, 200.3 g) and 18-crown-6 (2.64 g) were added to the solution, which was then stirred for 5 min. 1-Bromo-4-ethyl-4-(triethylsilyloxy)hexane (25.91 g) was then added to the mixture and reacted for 3.5 hours. After stopping the reaction by adding a saturated aqueous ammonium chloride solution, the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, filtered and the filtrate was evaporated under reduced pressure to remove the solvent. The resulting residue was purified by column chromatography (hexane:ethyl acetate=50:1) to give the titled compound (15.8 g).

Aufarbeitung

  1. additionwere added to the solution, which
  2. customreacted for 3.5 hours
  3. customthe reaction
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customthe filtrate was evaporated under reduced pressure
  8. customto remove the solvent
  9. customThe resulting residue was purified by column chromatography (hexane:ethyl acetate=50:1)

Quellen und Nachweise

ORD-Eintrag
ord-851c9b370e384106b3146c8a63abe960
Quelldatensatz
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07074777B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion