Dimethylformamide → 4-(4-Bromobutyl)-2,2-dimethyl-1,3-dioxolane

HRID 1577695Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1577695
[CH3:1][C:2]1([CH3:22])[O:6][CH:5]([CH2:7][CH2:8][CH2:9][CH2:10]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:4][O:3]1.CN(C)C=O.[Br-:28].[Li+]>O>[Br:28][CH2:10][CH2:9][CH2:8][CH2:7][CH:5]1[CH2:4][O:3][C:2]([CH3:22])([CH3:1])[O:6]1

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 82050Lithium BromideHCID 127708652,2-Dimethyl-4-(4-p-toluenesulfonyloxybutyl)-1,3-dioxolane

Produkt 1

HCID 46572524-(4-Bromobutyl)-2,2-dimethyl-1,3-dioxolane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a stirred solution of 220 g. of 2,2-dimethyl-4-(4-p-toluenesulfonyloxybutyl)-1,3-dioxolane in 800 ml. of dimethylformamide at 0° C. is added 115 g. of anhydrous lithium bromide in portions during 5 minutes. The resulting mixture is stirred at ambient temperature for 22 hours, diluted with water, and extracted with ether. The extract is washed with sodium bicarbonate solution, water, and brine; dried over magnesium sulfate; and concentrated. The residue is distilled to give a colorless liquid, b.p. 71°-74° C. (0.2 mm.).

Aufarbeitung

  1. extractionextracted with ether
  2. washThe extract is washed with sodium bicarbonate solution, water, and brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationand concentrated
  5. distillationThe residue is distilled
  6. customto give a colorless liquid, b.p. 71°-74° C. (0.2 mm.)

Quellen und Nachweise

ORD-Eintrag
ord-5d0e834004b8468080fd7cac9fc82160
Quelldatensatz
uspto-grants-1981_09
Patentnummer
US04288633

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