反应详情

5-(1-Fluoro-2-piperazin-1-ylethyl)-4-methyl-2-benzofuran-1(3H)-one hydrochloride (30 mg, 0.11 mmol), 2-(methyloxy)-4-(2-oxoethyl)benzonitrile (37 mg, 0.22 mmol), sodium cyanoborohydride (67 mg, 1.078 mmol) were added to a 25 mL flask containing a stir bar; to the flask was added MeOH (3 mL) and few drops of AcOH. The reaction mixture was subsequently stirred for 12 h r; LC indicated that reaction had gone to completion. The solution was concentrated to dryness, redissolved in EtOAc (15 mL) and washed with aq. NaHCO3 and aq. NaCl. The organic phase was dried over Na2SO4, filtered and concentrated to dryness. It was then re-dissolved in MeOH (3.5 mL) again, filtered and shot into mass-directed HPLC for separation to give the desired product. LC-MS (IE, m/z): 450 [M+1]+.

1. additioncontaining a stir bar
2. customLC indicated that reaction
3. concentrationThe solution was concentrated to dryness
4. dissolutionredissolved in EtOAc (15 mL)
5. washwashed with aq. NaHCO3 and aq. NaCl
6. dry with materialThe organic phase was dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated to dryness
9. dissolutionIt was then re-dissolved in MeOH (3.5 mL) again
10. filtrationfiltered
11. customshot into mass-directed HPLC for separation