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Ammonium Chloride → methyl (E,E,E)-7-[1-(1-methylethyl)-1,2,3,4-tetrahydroquinolin-6-yl]-3-methylocta-2,4,6-trienoate

HRID 2229171
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2229171
[Na].C[O-].[Na+].C[CH2:6][O:7][C:8](/[CH:10]=[C:11](/[CH2:13]P(OCC)(OCC)=O)\[CH3:12])=[O:9].[CH3:22][CH:23]([N:25]1[C:34]2[C:29](=[CH:30][C:31](/[C:35](/[CH3:39])=[CH:36]/[CH:37]=O)=[CH:32][CH:33]=2)[CH2:28][CH2:27][CH2:26]1)[CH3:24].[Cl-].[NH4+]>CO>[CH3:24][CH:23]([N:25]1[C:34]2[C:29](=[CH:30][C:31](/[C:35](/[CH3:39])=[CH:36]/[CH:37]=[CH:13]/[C:11](/[CH3:12])=[CH:10]/[C:8]([O:7][CH3:6])=[O:9])=[CH:32][CH:33]=2)[CH2:28][CH2:27][CH2:26]1)[CH3:22]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 6000084Ethyl 4-(diethoxyphosphoryl)-3-methylbut-2-enoateHCID 10490444(E)-3-[1-(1-methylethyl)-1,2,3,4-tetrahydroquinolin-6-yl]-2-butenalHCID 10942334Sodium Methoxide

Produkt 1

HCID 10569101
methyl (E,E,E)-7-[1-(1-methylethyl)-1,2,3,4-tetrahydroquinolin-6-yl]-3-methylocta-2,4,6-trienoate
Ausbeute 59,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

56 mg (2.46 mmol) of metallic sodium was added to methanol to prepare a methanolic solution of sodium methoxide. This solution was concentrated in a vacuum and suspended in N,N-dimethylformamide, followed by the addition of 560 mg (2.14 mmol) of triethyl 3-methyl-4-phosphonocrotonate under cooling with ice. After 30 minutes, 400 mg (1.64 mmol) of (E)-3-[1-(1-methylethyl)-1,2,3,4-tetrahydroquinolin-6-yl]-2-butenal was added to the mixture obtained above. The mixture thus obtained was stirred for one hour, followed by the addition of an aqueous solution of ammonium chloride. The obtained mixture was extracted with ethyl acetate. The organic phase was dried over anhydrous magnesium sulfate and concentrated in a vacuum. The obtained residue was purified by silica gel column chromatography (15% ethyl acetate/n-hexane) to give 330 mg of the title compound as a reddish-brown oil.

Aufarbeitung

  1. concentrationThis solution was concentrated in a vacuum
  2. temperatureunder cooling with ice
  3. customobtained above
  4. customThe mixture thus obtained
  5. extractionThe obtained mixture was extracted with ethyl acetate
  6. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated in a vacuum
  8. customThe obtained residue was purified by silica gel column chromatography (15% ethyl acetate/n-hexane)

Quellen und Nachweise

ORD-Eintrag
ord-c16aaa3df32b43b8912497d0d2706d4d
Quelldatensatz
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06420363B1

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