1,2-Dibromoethane → 1-(4-Chlorocinnamyl)-4-(5-isoquinolinesulfonyl)piperazine

1.31 g of the product of Example 172 was dissolved in 3 ml of dimethylformamide, to the solution were added 644 mg of 1,2-dibromoethane and 1.13 g of anhydrous potassium carbonate at a room temperature, and the mixture was stirred for 24 hours. After adding 100 ml of ethyl acetate, the ethyl acetate layer was sequentially washed with water and a saturated sodium chloride aqueous solution twice in each case, and dried over magnesium sulfate. The solution was filtered and evaporated under a reduced pressure, and resulting residue was purified on a silica gel column (silica gel 50 g, eluant: 5% methanol in chloroform), to obtain 356 mg of the title compound in a colorless amorphous form, while recovering the residual starting material.

1. washthe ethyl acetate layer was sequentially washed with water
2. dry with materiala saturated sodium chloride aqueous solution twice in each case, and dried over magnesium sulfate
3. filtrationThe solution was filtered
4. customevaporated under a reduced pressure
5. customresulting residue
6. customwas purified on a silica gel column (silica gel 50 g, eluant: 5% methanol in chloroform)

ORD record

ord-57a90189c8764512903a44bb9d37a3a5

Source dataset

uspto-grants-1993_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05245034