Sodium sulfate decahydrate → N-(3-Thienylmethyl)-9H-purin-6-amine

HRID 2413515Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2413515
[CH:1]1[S:5][CH:4]=[CH:3][C:2]=1[C:6]([NH:8][C:9]1[N:17]=[CH:16][N:15]=[C:14]2[C:10]=1[NH:11][CH:12]=[N:13]2)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[S:5]1[CH:4]=[CH:3][C:2]([CH2:6][NH:8][C:9]2[N:17]=[CH:16][N:15]=[C:14]3[C:10]=2[NH:11][CH:12]=[N:13]3)=[CH:1]1

Komponenten

6

Edukt 4

HCID 62649Sodium sulfate decahydrateHCID 166653HydrideHCID 13536441HCID 13536441, VerbindungHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 13536440N-(3-Thienylmethyl)-9H-purin-6-amineAusbeute 25 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A suspension of 20 g (0.082 mole) of 6-(3-thenoylamino)-purine in 1 l of absolute tetrahydrofuran is added dropwise to a stirred suspension of 6.5 g (0.17 mole) of lithium aluminum hydride in 350 ml of absolute tetrahydrofuran at 80° C. After 3 hours, the excess hydride is decomposed with sodium sulfate decahydrate, the residue is filtered off, the filtrate is brought to dryness and the resulting oily crystal slurry is crystallized several times from tetrahydrofuran. 6-(3-Thienylmethylamino)-purine is obtained in a yield of 25%.

Aufarbeitung

  1. filtrationthe residue is filtered off
  2. customthe resulting oily crystal slurry is crystallized several times from tetrahydrofuran

Quellen und Nachweise

ORD-Eintrag
ord-cf70309ff09a49eabf2c52b75795e070
Quelldatensatz
uspto-grants-1988_01
Patentnummer
US04718936

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