反応 #5832

反応方程式

pyridine

5-isoquinolinesulfonyl chloride hydrochloride

dimethylaminopyridine

water

→

title compound

3-(4-Chlorocinnamylamino)-2-(5-Isoquinolinesulfonylamino)Pyridine

反応条件

後処理

1. 1
   抽出extracted twice with 80 ml of chloroform
2. 2
   乾燥The extract was dried over magnesium sulfate
3. 3
   濃縮concentrated under a reduced pressure
4. 4
   その他resulting residue
5. 5
   洗浄eluted with chloroform/methanol (100:1)
6. 6
   その他resulting crystals
7. 7
   洗浄was washed with ethyl acetate

実験手順

4.52 g of the crystals obtained in Reference Example 41 was dissolved in 50 ml of pyridine, to the solution were added 5.8 g of 5-isoquinolinesulfonyl chloride hydrochloride and 3 g of dimethylaminopyridine, and the mixture was stirred for 18 hours at a room temperature, after adding 150 ml of water, extracted twice with 80 ml of chloroform. The extract was dried over magnesium sulfate and concentrated under a reduced pressure, and resulting residue was applied to a silica gel column and eluted with chloroform/methanol (100:1), and resulting crystals was washed with ethyl acetate, to obtain 1.2 g of the title compound as yellow crystals.

出典