Reaktion #1177746

Reaktionsgleichung

amorphous compound

1-[N,O-bis(5-isoquinolinesulphonyl) tyrosyl]-4-(3-phenylpropyl)piperazine

potassium hydroxide

sodium chloride

→

title compound

Ausbeute 46.0%

1-[N-(5-Isoquinolinesulfonyl) tyrosyl]-4-(3-phenylpropyl)piperazine

Ausbeute 46.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was refluxed for 10 hours
2. 2
   Extraktionextracted twice with 20 ml of a mixed solvent of chloroform/isopropanol (5:1)
3. 3
   TrocknenThe extract was dried over magnesium sulfate
4. 4
   Einengenconcentrated under a reduced pressure
5. 5
   Wascheneluted with chloroform/methanol (40:1 to 10:1)

Vorschrift

216 mg of the amorphous compound obtained in Example 32 was dissolved in 3 ml of methanol, and to the solution was added 0.6 ml of 2N potassium hydroxide aqueous solution. The mixture was refluxed for 10 hours, and after the addition of 30 ml of saturated sodium chloride aqueous solution, extracted twice with 20 ml of a mixed solvent of chloroform/isopropanol (5:1). The extract was dried over magnesium sulfate and concentrated under a reduced pressure, and a resulting residue was applied to a silica gel column and eluted with chloroform/methanol (40:1 to 10:1) to obtain 74 mg of the title compound in a colorless amorphous form.

Quelle