Potassium Hydroxide → HCID 131711586, Verbindung

HRID 972030

Reaktionsgleichung

Reaktionsgleichung von HRID 972030
[CH3:1][C:2]1([CH3:16])[NH:13][C:12]([CH3:15])([CH3:14])[CH2:11][C:4]2([NH:8][C:7](=[O:9])[NH:6][C:5]2=[O:10])[CH2:3]1.[O:17]1[CH2:28][CH:18]1[CH2:19][O:20][CH2:21][CH2:22][O:23][CH2:24][CH:25]1[O:27][CH2:26]1.[OH-:29].[K+]>CO>[OH:17][CH:18]([CH2:28][N:6]1[C:5](=[O:29])[C:4]2([CH2:3][C:2]([CH3:1])([CH3:16])[NH:13][C:12]([CH3:15])([CH3:14])[CH2:11]2)[NH:8][C:7]1=[O:9])[CH2:19][O:20][CH2:21][CH2:22][O:23][CH2:24][CH:25]([OH:27])[CH2:26][N:6]1[C:5](=[O:10])[C:4]2([CH2:3][C:2]([CH3:16])([CH3:1])[NH:13][C:12]([CH3:15])([CH3:14])[CH2:11]2)[NH:8][C:7]1=[O:9]

Komponenten

5

Edukt 3

HCID 14797Potassium HydroxideHCID 16683Glycol diglycidyl etherHCID 12680667,7,9,9-Tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

Produkt 1

HCID 131711586HCID 131711586, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 7.7 g of 7,7,9,9-tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione, 2.5 g of ethylene glycol bis(2,3-epoxypropyl)ether and 0.1 g of potassium hydroxide in 80 ml of methanol was refluxed for 11 hours. Insoluble materials were then filtered off and the filtrate was washed with hot methanol. The solution was dried and then the solvent evaporated off. The residue was recrystallised from N,N-dimethylformamide, giving the desired compound in the form of white crystals, melting at 262°-264° C.

Aufarbeitung

  1. temperaturewas refluxed for 11 hours
  2. filtrationInsoluble materials were then filtered off
  3. washthe filtrate was washed with hot methanol
  4. customThe solution was dried
  5. customthe solvent evaporated off
  6. customThe residue was recrystallised from N,N-dimethylformamide

Quellen und Nachweise

ORD-Eintrag
ord-8cdc1f6f705c4407b4c0af05e71bd929
Quelldatensatz
uspto-grants-1979_07
Patentnummer
US04162246

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