Reaktion #1932355

Reaktionsgleichung

4′-methyl-5-((2-methylpyrimidin-5-yl)methylcarbamoyl)biphenyl-3-carboxylic acid

N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride

1-hydroxybenzotriazole hydrate

hexahydro-1H-azepine

N,N-diisopropylethylamine

→

5-(Azepane-1-carbonyl)-4′-methyl-N-((2-methylpyrimidin-5-yl)methyl)biphenyl-3-carboxamide

Lösungsmittel

CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated in vacuo
2. 2
   SonstigeThe residue was purified by preparative HPLC (100×21.2 mm C18 column, 30-70% MeCN/water[10 mM Et2NH])
3. 3
   Sonstigeto yield a white foam

Vorschrift

To a mixture of 4′-methyl-5-((2-methylpyrimidin-5-yl)methylcarbamoyl)biphenyl-3-carboxylic acid (11 mg, 0.030 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (12 mg, 0.061 mmol), 1-hydroxybenzotriazole hydrate (4.7 mg, 0.030 mmol), and CH2Cl2 (2 mL) were added hexahydro-1H-azepine (4.5 mg, 0.046 mmol) and N,N-diisopropylethylamine (11 μL, 0.061 mmol). The mixture was stirred at room temperature overnight, and then concentrated in vacuo. The residue was purified by preparative HPLC (100×21.2 mm C18 column, 30-70% MeCN/water[10 mM Et2NH]) to yield a white foam.

Quelle