tert-Butyl piperazine-1-carboxylate → HCID 22730669, Verbindung

HRID 1785852Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1785852
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH2:9][CH:10]=O)[CH:6]=[CH:5][C:4]=1[C:12]1[CH:17]=[CH:16][C:15]([C:18]([O:20][CH3:21])=[O:19])=[CH:14][CH:13]=1.[N:22]1([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCCl>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH2:9][CH2:10][N:25]2[CH2:26][CH2:27][N:22]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:23][CH2:24]2)[CH:6]=[CH:5][C:4]=1[C:12]1[CH:13]=[CH:14][C:15]([C:18]([O:20][CH3:21])=[O:19])=[CH:16][CH:17]=1

Komponenten

5

Edukt 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 5049666Sodium triacetoxyborohydrideHCID 22730192HCID 22730192, Verbindung

Produkt 1

HCID 22730669HCID 22730669, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

A solution of Example 491C (400 mg, 1.41 mmol) and tert-butyl 1-piperazinecarboxylate (289 mg, 1.55 mmol) in 1,2-dichloroethane (5mL) at room temperature was treated with sodium triacetoxyborohydride (329 mg, 1.55 mmol), and stirred for 16 hours. The solution was purified by flash column chromatography on silica gel with 90:10:0.25 dichloromethane/methanol/concentrated ammonium hydroxide to provide the desired product.

Aufarbeitung

  1. customThe solution was purified by flash column chromatography on silica gel with 90:10:0.25 dichloromethane/methanol/concentrated ammonium hydroxide

Quellen und Nachweise

ORD-Eintrag
ord-463b713c69c341fd8ab16bd434ac5757
Quelldatensatz
uspto-grants-2009_03
Patentnummer
US07504512B2

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