Potassium Hydroxide → HCID 19738531, Verbindung

HRID 1460769Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1460769
[CH3:1][O:2][CH:3]([O:11][CH3:12])[CH2:4][NH:5][C:6](=[O:10])[O:7][CH2:8][CH3:9].[OH-].[K+].[Cl:15][C:16](=[CH2:19])[CH2:17]I>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.C1(C)C=CC=CC=1>[Cl:15][C:16](=[CH2:17])[CH2:19][N:5]([CH2:4][CH:3]([O:2][CH3:1])[O:11][CH3:12])[C:6](=[O:10])[O:7][CH2:8][CH3:9]

Komponenten

6

Edukt 3

HCID 14797Potassium Hydroxide2×HCID 10921057Ethyl 2,2-dimethoxyethylcarbamateHCID 109435662-Chloro-3-iodoprop-1-ene2×

Produkt 1

HCID 19738531HCID 19738531, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 66133Benzyl triethylammonium chlorideKatalysator2×HCID 1140TolueneLösungsmittel

Versuchsvorschrift

115 g (0.65 mol) of ethyl N-(2,2-dimethoxyethyl) -carbamate, 130 g of powdered potassium hydroxide and 2 g of triethylbenzylammonium chloride are initially introduced into 650 ml of toluene and 142 g (0.7 mol) of 2-chloroallyl iodide are added dropwise at room temperature. After stirring overnight, a gas chromatogram showed incomplete conversion, hence 65 g of powdered potassium hydroxide and 1 g of triethylbenzylammonium chloride were added again and a further 71 g (0.35 mol) of 2-chloroallyl iodide were added dropwise. After stirring overnight at room temperature, the salts were filtered off with suction, the filtrate was washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated, and the residue was distilled.

Aufarbeitung

  1. additionare added dropwise at room temperature
  2. additionwere added again
  3. stirringAfter stirring overnight at room temperature
  4. filtrationthe salts were filtered off with suction
  5. washthe filtrate was washed with saturated sodium chloride solution
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated
  8. distillationthe residue was distilled

Quellen und Nachweise

ORD-Eintrag
ord-d644888567ac42bcaee13a3a4e19dfe0
Quelldatensatz
uspto-grants-1991_12
Patentnummer
US05071999

Notizen zur Reaktion

Wird geladen…