Sodium Hydroxide → HCID 178456515, Verbindung

HRID 480151Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 480151
[O:1]=[C:2]1[N:10]([CH2:11][CH2:12][CH3:13])[C:9]2[N:8]=[C:7]([C:14]34[CH2:21][CH2:20][C:17]([CH2:22][CH2:23][C:24]5[N:28](CCC#N)[N:27]=[N:26][N:25]=5)([CH2:18][CH2:19]3)[CH2:16][CH2:15]4)[NH:6][C:5]=2[C:4](=[O:33])[N:3]1[CH2:34][CH2:35][CH3:36].[OH-].[Na+]>C1COCC1>[CH2:34]([N:3]1[C:4](=[O:33])[C:5]2[NH:6][C:7]([C:14]34[CH2:15][CH2:16][C:17]([CH2:22][CH2:23][C:24]5[NH:28][N:27]=[N:26][N:25]=5)([CH2:18][CH2:19]3)[CH2:20][CH2:21]4)=[N:8][C:9]=2[N:10]([CH2:11][CH2:12][CH3:13])[C:2]1=[O:1])[CH2:35][CH3:36]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 18767693HCID 18767693, Verbindung

Produkt 1

HCID 178456515HCID 178456515, VerbindungAusbeute 41,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 3-(5-{2-[4-(2,6-Dioxo-1,3-dipropyl-2,3,6,7-tetrahydro-1H-purin-8-yl)-bicyclo[2.2.2]oct-1-yl]-ethyl}-tetrazol-1-yl)-propionitrile (150 mg, 0.30 mmol) in THF (20 ml) was added 3 ml of 1N NaOH. The resulting mixture was stirred at rt for 8 h, concentrated in vacuo and extracted with CH2Cl2 (2×10 ml). The aqueous phase was acidified by the careful addition of concentrated HCl and the resulting precipitate was collected, washed with water and dried to afford 55 mg (41%) of a white powder. MS: 441 (MH+).

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. extractionextracted with CH2Cl2 (2×10 ml)
  3. additionThe aqueous phase was acidified by the careful addition of concentrated HCl
  4. customthe resulting precipitate was collected
  5. washwashed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-cb1e9ecbff5043809d74c04bdb8e9aa7
Quelldatensatz
uspto-grants-2003_11
Patentnummer
US06649600B1

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