반응 #5827

반응 방정식

sodium bicarbonate

amorphous compound

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

sodium hydroxide

citric acid

→

title compound

수율 74.7%

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

수율 74.7%

용매

methanol

methanol

tetrahydrofuran

반응 조건

후처리

1. 1
   온도the mixture was refluxed for 2 hours
2. 2
   온도cooled
3. 3
   기타resulting insoluble matter
4. 4
   추출the solution was extracted twice with 400 ml of chloroform
5. 5
   건조The extract was dried over magnesium sulfate
6. 6
   기타evaporated
7. 7
   기타to remove the solvent under a reduced pressure
8. 8
   기타resulting residue
9. 9
   세척eluted with chloroform/methanol (20:1)

실험 절차

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.

출처