Benzyl Chloride → HCID 18338481, Verbindung

HRID 2298439Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2298439
[CH2:1](Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[NH:15]1[CH2:20][CH2:19][CH:18]([CH2:21][CH:22]([C:28]([O:30][CH2:31][CH3:32])=[O:29])[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH2:17][CH2:16]1>C(O)(=O)C>[CH2:1]([N:15]1[CH2:16][CH2:17][CH:18]([CH2:21][CH:22]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:28]([O:30][CH2:31][CH3:32])=[O:29])[CH2:19][CH2:20]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Reaktionsbedingungen

Temperatur
62.5 °C

Versuchsvorschrift

Benzyl chloride (54.4 g) and sodium carbonate (149.4 g) were added to the solution of the acetic acid salt of diethyl (4-piperidylmethyl)malonate [XXIXb] from the previous step. The obtained slurry was stirred for 12 hours at 60-65° C. and evaporated under reduced pressure. Water was added to the residue and the obtained mixture was extracted with dichloromethane. The organic layer was washed with water, dried over sodium sulfate, passed through short silica gel column and evaporated under reduced pressure. The obtained residue was washed with hexanes and dried under reduced pressure to give diethyl (N-benzyl-4-piperidylmethyl)malonate [XXIIb].

Aufarbeitung

  1. customevaporated under reduced pressure
  2. additionWater was added to the residue
  3. extractionthe obtained mixture was extracted with dichloromethane
  4. washThe organic layer was washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. washThe obtained residue was washed with hexanes
  8. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-17333962149b4873b781260e413c8c90
Quelldatensatz
uspto-grants-2002_12
Patentnummer
US06492522B1

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