Water → 1-Oxa-4-azaspiro[4.5]decane-3,3-dimethanol

HRID 1703747Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1703747
[OH:1][CH2:2][C:3]([CH2:7][OH:8])([CH2:5][OH:6])[NH2:4].[C:9]1(=O)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.O>C1(C)C=CC=CC=1>[CH2:2]([C:3]1([CH2:7][OH:8])[NH:4][C:9]2([CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]2)[O:6][CH2:5]1)[OH:1]

Komponenten

5

Edukt 3

HCID 962WaterHCID 6503Tris(hydroxymethyl)aminomethaneHCID 7967Cyclohexanone

Produkt 1

HCID 3251041-Oxa-4-azaspiro[4.5]decane-3,3-dimethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

Tris-(hydroxymethyl)-aminomethane (24.23 grams; 0.2 mole) and cyclohexanone (19.63 grams; 0.2 mole) were refluxed overnight in 150 mls of toluene, using a water separator to remove approximately 3.6 mls of water. The toluene was then removed by distillation and the residue was recrystallized from acetone to obtain 32 grams (79.5% of theoretical; m.p. 117°-119° C.) of the desired compound.

Aufarbeitung

  1. customto remove approximately 3.6 mls of water
  2. customThe toluene was then removed by distillation
  3. customthe residue was recrystallized from acetone

Quellen und Nachweise

ORD-Eintrag
ord-71476f08ce7e4592912d35338c49f52f
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04125518

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