Reaktion #5832

Reaktionsgleichung

pyridine

5-isoquinolinesulfonyl chloride hydrochloride

dimethylaminopyridine

water

→

title compound

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

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted twice with 80 ml of chloroform
2. 2
   TrocknenThe extract was dried over magnesium sulfate
3. 3
   Einengenconcentrated under a reduced pressure
4. 4
   Sonstigeresulting residue
5. 5
   Wascheneluted with chloroform/methanol (100:1)
6. 6
   Sonstigeresulting crystals
7. 7
   Waschenwas washed with ethyl acetate

Vorschrift

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.

Quelle