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Potassium Iodide → HCID 57115188, Verbindung

HRID 648635
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 648635
[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[CH:13]([CH:15]([C:24]([NH2:26])=[O:25])[C:16]2[CH:23]=[CH:22][C:19]([CH2:20]Cl)=[CH:18][CH:17]=2)[CH3:14])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.S(Cl)(Cl)=O.[CH2:31]([O:33][C:34](=[O:41])[CH2:35][C:36]([O:38][CH2:39][CH3:40])=[O:37])[CH3:32].[Na].[Na].C(OC(=O)CC(OCC)=O)C.[I-].[K+]>C(Cl)(Cl)Cl.C(O)C>[CH2:31]([O:33][C:34](=[O:41])[CH:35]([CH2:20][C:19]1[CH:22]=[CH:23][C:16]([CH:15]([CH:13]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)[CH3:14])[C:24]([NH2:26])=[O:25])=[CH:17][CH:18]=1)[C:36]([O:38][CH2:39][CH3:40])=[O:37])[CH3:32]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 4875Potassium IodideHCID 7761Diethyl MalonateHCID 24386Thionyl ChlorideHCID 5360545SodiumHCID 20145263HCID 20145263, VerbindungHCID 86602522HCID 86602522, Verbindung

Produkt 1

HCID 57115188
HCID 57115188, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A solution of 3.7 gm (10 m mol) of 4-[(1-(2-piperidinophenyl)-ethyl)-aminocarbonylmethyl]-benzyl chloride [m.p.: 123°-125° C.; prepared from the alcohol described in Example 25 by means of thionyl chloride in chloroform] in 35 ml of absolute ethanol was added dropwise to a solution of sodium malonic acid diethyl ester [prepared from 0.7 gm (30 m mol) of sodium in 25 ml of absolute ethanol and 4.8 gm (30 m mol) of malonic acid diethyl ester]. A catalytic amount of potassium iodide was added, and the mixture was refluxed for 16 hours. After evaporation in vacuo, the evaporation residue was adjusted neutral by means of hydrochloric acid and extracted with methylene chloride. The organic extract was dried over sodium sulfate, filtered, and evaporated in vacuo. The evaporation residue was purified by column chromatography on silica gel (toluene/acetone=6:1).

Aufarbeitung

  1. temperaturethe mixture was refluxed for 16 hours
  2. customAfter evaporation in vacuo
  3. extractionextracted with methylene chloride
  4. extractionThe organic extract
  5. dry with materialwas dried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. customThe evaporation residue was purified by column chromatography on silica gel (toluene/acetone=6:1)

Quellen und Nachweise

ORD-Eintrag
ord-7626ae9b2c334a888574a9918efee351
Quelldatensatz
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04735959

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