Hydrochloric Acid → 7-oxa-1,3-diazaspiro[4.4]nonane-2,4-dione

HRID 2058946Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2058946
[C:1](=[O:4])([O-])[O-].[NH4+:5].[NH4+:6].O=[C:8]1[CH2:12][CH2:11][O:10][CH2:9]1.[C-]#N.[K+].Cl.[CH2:17]([OH:19])C>O>[NH:5]1[C:8]2([CH2:12][CH2:11][O:10][CH2:9]2)[C:17](=[O:19])[NH:6][C:1]1=[O:4]

Komponenten

7

Edukt 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 9032Potassium CyanideHCID 517111Ammonium CarbonateHCID 5293923-Oxotetrahydrofuran

Produkt 1

HCID 5436707-oxa-1,3-diazaspiro[4.4]nonane-2,4-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Versuchsvorschrift

A solution of 19.2 g of ammonium carbonate in 42 ml of ethanol and 28 ml of water is added to 10.0 g of 3-ketotetrahydrofuran. The resulting mixture is heated to 55° and to it is then added, dropwise, a solution of 6.3 g of potassium cyanide in 15 ml of water. The reaction mixture is stirred at 55° for 18 hrs. Thereafter the reaction mixture is evaporated in vacuo to dryness to obtain a residue. The residue is dissolved in a minimum of water and the mixture made acidic with 2 N hydrochloric acid. The first crop of the title product precipitates out on cooling and is filtered off. A second crop of the title product is obtained by concentrating the filtrate and cooling. The two combined crops are recrystalized from ethanol to give refined title product, m.p. 202°-204°.

Aufarbeitung

  1. temperatureThe resulting mixture is heated to 55° and to it
  2. additionis then added
  3. customThereafter the reaction mixture is evaporated in vacuo to dryness
  4. customto obtain a residue
  5. customThe first crop of the title product precipitates out
  6. temperatureon cooling
  7. filtrationis filtered off

Quellen und Nachweise

ORD-Eintrag
ord-eb82410f819b4304965ed1b08c21219b
Quelldatensatz
uspto-grants-1982_03
Patentnummer
US04320135

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