反应详情

4-Methyl-5-[1-(methyloxy)-2-piperazin-1-ylethyl]-2-benzofuran-1(3H)-one hydrochloride (50 mg, 0.17 mmol), 2-(methyloxy)-4-(2-oxoethyl)benzonitrile (60 mg, 0.34 mmol), sodium cyanoborohydride (108 mg, 1.72 mmol) and a stir bar were added to a 25 mL flask and few drops of AcOH. The resulting mixture was then dissolved in MeOH (3 mL) and stirred for 12 h; analysis by LC indicated that reaction had gone to completion. The reaction mixture was treated with EtOAc (20 mL) and washed with aq. NaHCO3, aq. NaCl. The organic phase was then dried over Na2SO4, filtered and concentrated to dryness; the resulting residue was then dissolved in MeOH (3.5 mL), filtered and shot into Mass-directed HPLC for separation to give the desired product. LC-MS (IE, m/z): 481 [M+1]+.

1. customanalysis by LC indicated that reaction
2. washwashed with aq. NaHCO3, aq. NaCl
3. dry with materialThe organic phase was then dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated to dryness
6. dissolutionthe resulting residue was then dissolved in MeOH (3.5 mL)
7. filtrationfiltered
8. customshot into Mass-directed HPLC for separation