反应详情

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.

1. extractionextracted twice with 80 ml of chloroform
2. dry with materialThe extract was dried over magnesium sulfate
3. concentrationconcentrated under a reduced pressure
4. customresulting residue
5. washeluted with chloroform/methanol (100:1)
6. customresulting crystals
7. washwas washed with ethyl acetate