反应 #5819

反应方程式

amorphous compound

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

potassium hydroxide

sodium chloride

→

title compound

收率 46.0%

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

收率 46.0%

溶剂

methanol

反应条件

后处理

1. 1
   温度The mixture was refluxed for 10 hours
2. 2
   萃取extracted twice with 20 ml of a mixed solvent of chloroform/isopropanol (5:1)
3. 3
   干燥The extract was dried over magnesium sulfate
4. 4
   浓缩concentrated under a reduced pressure
5. 5
   洗涤eluted with chloroform/methanol (40:1 to 10:1)

实验过程

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.

来源