Sodium hydride → HCID 66674083, Verbindung

HRID 421810

Reaktionsgleichung

Reaktionsgleichung von HRID 421810
[CH:1]1([C:7]([C:9]2[CH:10]([C:27]3[CH:34]=[CH:33][C:30]([C:31]#[N:32])=[CH:29][CH:28]=3)[NH:11][C:12](=[O:26])[N:13]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:24])[F:23])[CH:17]=3)[C:14]=2[CH3:15])=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].Br[CH2:38][CH2:39][N:40]([CH2:43][CH3:44])[CH2:41][CH3:42]>C1COCC1>[CH:1]1([C:7]([C:9]2[CH:10]([C:27]3[CH:28]=[CH:29][C:30]([C:31]#[N:32])=[CH:33][CH:34]=3)[N:11]([CH2:38][CH2:39][N:40]([CH2:43][CH3:44])[CH2:41][CH3:42])[C:12](=[O:26])[N:13]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([F:25])([F:23])[F:24])[CH:17]=3)[C:14]=2[CH3:15])=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

5

Edukt 3

HCID 24758Sodium hydrideHCID 706082-Bromo-N,N-diethylethanamineHCID 59684783HCID 59684783, Verbindung

Produkt 1

HCID 66674083HCID 66674083, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a stirred solution of Example 21 (780 mg, 1.67 mmol) in THF (25 ml) is added sodium hydride (60% dispersion in mineral oil; 653 mg, 2.53 mmol). The mixture is stirred for 1 hour at room temperature, then 2-bromo-N,N-diethylethanamine (653 mg, 2.53 mmol) is added, and the solution is stirred overnight (16 h) at room temperature. The reaction mixture is quenched with methanol (10 ml), concentrated, and the crude product is purified by preparative HPLC.

Aufarbeitung

  1. stirringthe solution is stirred overnight (16 h) at room temperature
  2. customThe reaction mixture is quenched with methanol (10 ml)
  3. concentrationconcentrated
  4. customthe crude product is purified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-687052fa5a1d4a5e90cd74506f7ac943
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101615B2

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