Acetal → 1,3,5-Triazine-2,4-diamine, 3,6-dihydro-N2,N2,6-trimethyl-, hydrochloride (1:1)

HRID 874151

Reaktionsgleichung

Reaktionsgleichung von HRID 874151
[CH3:1][N:2]([C:4]([N:6]=[C:7]([NH2:9])[NH2:8])=[NH:5])[CH3:3].[ClH:10].[CH2:11](OC(OCC)C)[CH3:12]>C(O)C(C)C.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[ClH:10].[NH2:8][C:7]1[NH:6][C:4]([N:2]([CH3:3])[CH3:1])=[N:5][CH:11]([CH3:12])[N:9]=1

Komponenten

5

Edukt 2

HCID 7765AcetalHCID 14219Metformin Hydrochloride

Produkt 1

HCID 101764861,3,5-Triazine-2,4-diamine, 3,6-dihydro-N2,N2,6-trimethyl-, hydrochloride (1:1)Ausbeute 77,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 521998p-Toluenesulfonic acid monohydrateKatalysatorHCID 6560IsobutanolLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

Comparative experiment) A mixture of 250.2 g of metformin hydrochloride, 213.6 g of acetaldehyde diethyl acetal and 12.5 g of toluene-4-sulfonic acid monohydrate in 500 ml of isobutanol was heated under reflux for 40 hours. Some of the solvent was removed by distillation. The mixture was cooled to 10° C., and the white precipitate was separated off, giving 224.7 g (77.4%) of 4-amino-3,6-dihydro-2-dimethylamino-6-methyl-1,3,5-triazine hydrochloride.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 40 hours
  3. customSome of the solvent was removed by distillation
  4. customthe white precipitate was separated off

Quellen und Nachweise

ORD-Eintrag
ord-c879830670284ceba19d166f8c268531
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08980828B2

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