Chlorotrimethylsilane → HCID 56624785, Verbindung

HRID 65388Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 65388
[Cl:1][CH:2]([Cl:12])[C:3]([N:5]1[CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]1)=[O:4].[CH2:13](O)[CH2:14][CH2:15][OH:16].C[Si](C)(C)Cl>>[CH2:15]1[O:16][C:8]2([CH2:7][CH2:6][N:5]([C:3](=[O:4])[CH:2]([Cl:1])[Cl:12])[CH2:10][CH2:9]2)[O:11][CH:14]1[CH3:13]

Komponenten

4

Edukt 3

HCID 6397ChlorotrimethylsilaneHCID 104421,3-PropanediolHCID 130182281-(Dichloroacetyl)piperidin-4-one

Produkt 1

HCID 56624785HCID 56624785, VerbindungAusbeute 66,6 %

Versuchsvorschrift

A mixture of 19 g (0.09 mol) of N-dichloroacetylpiperid-4-one, 7.5 g (0.099 mol) of propane-1,3-diol and 22.4 g (0.21 mol) of trimethylchlorosilane was boiled under reflux for 12 hours, while stirring. Thereafter, the reaction mixture was concentrated under reduced pressure and the residue was then subjected to brief incipient distillation under greatly reduced pressure. The resulting brown oil, which slowly crystallized completely, was recrystallized from 200 ml of toluene. 16 g (66.6% of theory) of N-dichloroacetyl-piperid-4-one propylene ketal of melting point 115° C. were obtained.

Aufarbeitung

  1. temperatureunder reflux for 12 hours
  2. concentrationThereafter, the reaction mixture was concentrated under reduced pressure
  3. distillationthe residue was then subjected to brief incipient distillation under greatly reduced pressure
  4. customThe resulting brown oil, which slowly crystallized completely
  5. customwas recrystallized from 200 ml of toluene

Quellen und Nachweise

ORD-Eintrag
ord-39fcff8cd157445eaa6313081d773d75
Quelldatensatz
uspto-grants-1986_09
Patentnummer
US04614537

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