Reaktion #1674367

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 2 N 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