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Hydrochloric Acid → 6-Amino-2-[(2-cyclopropylethyl)oxy]-9-(tetrahydro-2H-pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one

HRID 1011186
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1011186
[CH:1]1([CH2:4][CH2:5][O:6][C:7]2[N:15]=[C:14]3[C:10]([N:11]=[C:12]([O:23]C)[N:13]3[CH2:16][CH:17]3[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)=[C:9]([NH2:25])[N:8]=2)[CH2:3][CH2:2]1.Cl.[OH-].[Na+]>CO.O1CCOCC1.O>[NH2:25][C:9]1[N:8]=[C:7]([O:6][CH2:5][CH2:4][CH:1]2[CH2:3][CH2:2]2)[N:15]=[C:14]2[C:10]=1[NH:11][C:12](=[O:23])[N:13]2[CH2:16][CH:17]1[CH2:18][CH2:19][O:20][CH2:21][CH2:22]1
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Komponenten

7

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 576997352-[(2-Cyclopropylethyl)oxy]-8-(methyloxy)-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-Purin-6-amine

Produkt 1

HCID 576997106-Amino-2-[(2-cyclopropylethyl)oxy]-9-(tetrahydro-2H-pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-oneAusbeute 77,8 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887
Methanol
Lösungsmittel
2×
HCID 962WaterLösungsmittel
HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

2-[(2-Cyclopropylethyl)oxy]-8-(methoxy)-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine (0.1259 g) was dissolved in methanol (5 mL) and added 4N hydrogen chloride in 1,4-dioxane (2 mL). The reaction was stirred at room temperature for 4 hours. The reaction mixture was evaporated under reduced pressure to give a solid which was then suspended in water (1 mL) and small quantity of methanol (2-3 mL). This was then neutralised (to pH 7) by the addition of 2N sodium hydroxide. The suspension was evaporated to near dryness under reduced pressure and then suspended the solid in water (3 mL). The solid was filtered off under suction and washed with a few drops of methanol before being air-dried under suction. This material was then dried to constant weight under vacuo at 50° C. to give the title compound (94 mg).

Aufarbeitung

  1. customThe reaction mixture was evaporated under reduced pressure
  2. customto give a solid which
  3. customThe suspension was evaporated
  4. filtrationThe solid was filtered off under suction
  5. washwashed with a few drops of methanol
  6. custombefore being air-dried under suction
  7. customThis material was then dried to constant weight under vacuo at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-da2d59cc97ee47018348c530fe9111c8
Quelldatensatz
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07977344B2

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