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Benzaldehyde → Styryl[4-(4-fluorophenyl)piperazino] sulfone

HRID 1582050
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1582050
[Li+].CC([N-]C(C)C)C.C([Li])CCC.C(NC(C)C)(C)C.[F:21][C:22]1[CH:27]=[CH:26][C:25]([N:28]2[CH2:33][CH2:32][N:31]([S:34]([CH3:37])(=[O:36])=[O:35])[CH2:30][CH2:29]2)=[CH:24][CH:23]=1.C(OP(Cl)(OCC)=O)C.[CH:47](=O)[C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1>C1COCC1>[F:21][C:22]1[CH:23]=[CH:24][C:25]([N:28]2[CH2:33][CH2:32][N:31]([S:34](/[CH:37]=[CH:47]/[C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=3)(=[O:35])=[O:36])[CH2:30][CH2:29]2)=[CH:26][CH:27]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 240BenzaldehydeHCID 7912DiisopropylamineHCID 13139Diethyl chlorophosphateHCID 6690391-(4-Fluorophenyl)-4-(methylsulfonyl)piperazineHCID 2724682Lithium diisopropylamideHCID 178418339Butyllithium

Produkt 1

HCID 882266
Styryl[4-(4-fluorophenyl)piperazino] sulfone
Ausbeute 46,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel4×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

To a solution of LDA [8.5 mmol ; prepared by slow addition of n-butyl lithium (3.5 ml, 8.5 mmol, 2.5 M in hexane) to a solution of diisopropylamine (860 mg, 8.5 mmol) in dry THF (5 ml) at −78° C.] at −78° C. was added a solution of 1-(4-fluorophenyl)4-(methanesulfonyl)piperazine (1 g, 3.87 mmol) in THF (25 ml) dropwise. The mixture was stirred at −78° C. for 1 hour and a solution of diethylchlorophosphate (670 mg; 3.87 mmol) in THF (3 ml) was added. The mixture was stirred at −78° C. for 1 hour and benzaldehyde (450 mg; 4.24 mmol) in THF (3 ml) was added. The mixture was gently warmed to room temperature and stirred for 18 hours. The mixture was washed with aqueous ammonium chloride and extracted with ethyl acetate. The organic layers were washed with water, brine and dried over MgSO4. Purification of the residue on silica (eluant: dichloromethane) afforded 1-(4-fluorophenyl)4(trans-β-styrenesulfonyl)piperazine as a white powder (621 mg, 46%).

Aufarbeitung

  1. stirringThe mixture was stirred at −78° C. for 1 hour
  2. temperatureThe mixture was gently warmed to room temperature
  3. stirringstirred for 18 hours
  4. washThe mixture was washed with aqueous ammonium chloride
  5. extractionextracted with ethyl acetate
  6. washThe organic layers were washed with water, brine
  7. dry with materialdried over MgSO4
  8. customPurification of the residue on silica (eluant: dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-af3bcab8828840e69b146a71e8189780
Quelldatensatz
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06734184B1

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