تفاعل #5827

معادلة التفاعل

sodium bicarbonate

amorphous compound

1-Benzyloxycarbonyl-4-[N,O-Bis(5-Isoquinolinesulfonyl)Tyrosyl]Homopiperazine

sodium hydroxide

citric acid

→

title compound

المردود 74.7%

1-Benzyloxycarbonyl-4-[N-(5-Isoquinolinesulfonyl)Tyrosyl]Homopiperazine

المردود 74.7%

المذيبات

methanol

methanol

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was refluxed for 2 hours
2. 2
   درجة الحرارةcooled
3. 3
   أخرىresulting insoluble matter
4. 4
   استخلاصthe solution was extracted twice with 400 ml of chloroform
5. 5
   تجفيفThe extract was dried over magnesium sulfate
6. 6
   أخرىevaporated
7. 7
   أخرىto remove the solvent under a reduced pressure
8. 8
   أخرىresulting residue
9. 9
   غسيلeluted with chloroform/methanol (20:1)

الإجراء التجريبي

5.50 g of the amorphous compound obtained in Example 122 was dissolved in 30 ml of methanol and 30 ml of tetrahydrofuran, to the solution was added 60 ml of 1N sodium hydroxide, and the mixture was refluxed for 2 hours and then cooled. The reaction mixture was acidified with citric acid and then alkalized with sodium bicarbonate, resulting insoluble matter was dissolved with a small amount of methanol, and the solution was extracted twice with 400 ml of chloroform. The extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure, and resulting residue was applied to a silica gel column and eluted with chloroform/methanol (20:1) to obtain 3.1 g of the title compound in a colorless amorphous form.

المصدر