반응 #5819

반응 방정식

amorphous compound

1-[N,O-Bis(5-Isoquinolinesulphonyl)Tyrosyl]-4-(3-Phenylpropyl)Piperazine

potassium hydroxide

sodium chloride

→

title compound

수율 46.0%

1-[N-(5-Isoquinolinesulfonyl)Tyrosyl]-4-(3-Phenylpropyl)Piperazine

수율 46.0%

용매

methanol

반응 조건

후처리

1. 1
   온도The mixture was refluxed for 10 hours
2. 2
   추출extracted twice with 20 ml of a mixed solvent of chloroform/isopropanol (5:1)
3. 3
   건조The extract was dried over magnesium sulfate
4. 4
   농축concentrated under a reduced pressure
5. 5
   세척eluted with chloroform/methanol (40:1 to 10:1)

실험 절차

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.

출처