반응 #5832

반응 방정식

pyridine

5-isoquinolinesulfonyl chloride hydrochloride

dimethylaminopyridine

water

→

title compound

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

반응 조건

후처리

1. 1
   추출extracted twice with 80 ml of chloroform
2. 2
   건조The extract was dried over magnesium sulfate
3. 3
   농축concentrated under a reduced pressure
4. 4
   기타resulting residue
5. 5
   세척eluted with chloroform/methanol (100:1)
6. 6
   기타resulting crystals
7. 7
   세척was washed with ethyl acetate

실험 절차

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.

출처