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

HRID 1392136
Notes
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Reaction equation

HRID 1392136 reaction equation
[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
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

8

Reactant 6

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

Product 1

HCID 882266
Styryl[4-(4-fluorophenyl)piperazino] sulfone
Yield 46.3%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent4×

Conditions

Temperature
-78 °C

Procedure

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%).

Workup

  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)

Sources & evidence

ORD record
ord-e6e31bef8b7d4fe4949106e08c65badc
Source dataset
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07342020B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes