Iodine → 2-(2-Dimethylaminoethoxy)ethyl Methacrylate

HRID 582446

Reaktionsgleichung

Reaktionsgleichung von HRID 582446
[Mg].II.[CH3:4][N:5]([CH3:12])[CH2:6][CH2:7][O:8][CH2:9][CH2:10][OH:11].C1C2NC3C(=CC=CC=3)SC=2C=CC=1.[C:27](OC)(=[O:31])[C:28]([CH3:30])=[CH2:29]>CO>[C:27]([O:11][CH2:10][CH2:9][O:8][CH2:7][CH2:6][N:5]([CH3:12])[CH3:4])(=[O:31])[C:28]([CH3:30])=[CH2:29]

Komponenten

7

Edukt 5

HCID 807IodineHCID 6658Methyl MethacrylateHCID 7108PhenothiazineHCID 743482-(2-(Dimethylamino)ethoxy)ethanolHCID 5462224Magnesium

Produkt 1

HCID 158702902-(2-Dimethylaminoethoxy)ethyl Methacrylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

A magnesium methoxide solution was prepared by dissolving magnesium metal (4 g) in anhydrous methanol (100 ml) in the presence of a small amount of iodine (approximately 0.1 g). A portion of the resulting solution (18 ml) was placed in a 250 ml reaction vessel and then 2-(2-dimethylaminoethoxy)ethanol (23.6 g) was added, followed by the addition of phenothiazine (0.1 g) and methyl methacrylate (117 g). The mixture was stirred and heated until the methanol started to distill. When all of the methanol was collected, the mixture was cooled to room temperature and the solids were filtered off. The filtrate was subjected to fractionation under reduced pressure. The excess of methyl methacrylate was separated and then pure 2-(2-dimethylaminoethoxy)ethyl methacrylate was collected at 97-102° C./4 mmHg. Yield 22.1 g.

Aufarbeitung

  1. distillationto distill
  2. customWhen all of the methanol was collected
  3. filtrationthe solids were filtered off
  4. customThe excess of methyl methacrylate was separated
  5. custompure 2-(2-dimethylaminoethoxy)ethyl methacrylate was collected at 97-102° C./4 mmHg

Quellen und Nachweise

ORD-Eintrag
ord-d1ed5f33d9364e8cb4ab1b7b339ae5e7
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05925253

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