反応 #5827

反応方程式

sodium bicarbonate

amorphous compound

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

sodium hydroxide

citric acid

→

title compound

収率 74.7%

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

収率 74.7%

溶媒

methanol

methanol

tetrahydrofuran

反応条件

後処理

1. 1
   温度the mixture was refluxed for 2 hours
2. 2
   温度cooled
3. 3
   その他resulting insoluble matter
4. 4
   抽出the solution was extracted twice with 400 ml of chloroform
5. 5
   乾燥The extract was dried over magnesium sulfate
6. 6
   その他evaporated
7. 7
   その他to remove the solvent under a reduced pressure
8. 8
   その他resulting residue
9. 9
   洗浄eluted with chloroform/methanol (20:1)

実験手順

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.

出典