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Hydrazine hydrate (1:1) → 9-(3-Aminopropyl)-2-butoxy-8-methoxy-9H-purin-6-amine

HRID 2036348
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2036348
[NH2:1][C:2]1[N:10]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])[N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([O:30][CH3:31])[N:6]2[CH2:16][CH2:17][CH2:18][N:19]1C(=O)C2C(=CC=CC=2)C1=O.O.NN>C(O)C>[NH2:19][CH2:18][CH2:17][CH2:16][N:6]1[C:5]([O:30][CH3:31])=[N:4][C:3]2[C:7]1=[N:8][C:9]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])=[N:10][C:2]=2[NH2:1]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 582909572-[3-(6-Amino-2-butoxy-8-methoxy-9H-purin-9-yl)propyl]-1H-isoindole-1,3(2H)-dione

Produkt 1

HCID 231585469-(3-Aminopropyl)-2-butoxy-8-methoxy-9H-purin-6-amineAusbeute 65,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

2-{3-[6-Amino-2-(butyloxy)-8-(methyloxy)-9H-purin-9-yl]propyl}-1H-isoindole-1,3(2H)-dione (6.06 g, 14.28 mmol) was dissolved in ethanol (60 ml) and hydrazine monohydrate (6.00 ml) was added and stirred at ambient temperature for 10 hours. The resultant mixture was concentrated under reduced pressure and the residue suspended in DCM (100 ml) and stirred for 1 hour. The suspension was filtered, and the filtered solid washed with DCM (10 ml). The filtrate and washings were washed with water (50 ml) and dried. The organic solution was concentrated under reduced pressure to give the title compound as an off-white solid (2.74 g).

Aufarbeitung

  1. concentrationThe resultant mixture was concentrated under reduced pressure
  2. stirringstirred for 1 hour
  3. filtrationThe suspension was filtered
  4. washthe filtered solid washed with DCM (10 ml)
  5. washThe filtrate and washings were washed with water (50 ml)
  6. customdried
  7. concentrationThe organic solution was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-360a6d5f1aa141c2a2bf7d07b331b520
Quelldatensatz
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08575181B2

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