反应详情

To a stirred solution of 1-(2-oxoethyl)-3,4-dihydro-1H-2-benzopyran-6-carbonitrile (0.454 g, 2.26 mmol) in methanol (30 mL) was added (3R)-1-(6-fluoro-1-naphthyl)-3-methylpiperazine (0.61 g, 2.49 mmol), and the mixture stirred for 10 min. Sodium cyanoborohydride (0.157 g, 2.49 mmol) and acetic acid (0.25 mL) were added and the mixture stirred for 18 h. A further portion of sodium cyanoborohydride (0.20 g) was added and the reaction stirred for 6 h. The mixture was quenched with water, and the solvent removed in vacuo. Water was added and the mixture extracted with chloroform, the organic extracts dried (MgSO4), filtered and evaporated in vacuo. The crude product was purified by preparative LC-MS to yield the title compound as a yellow oil.

1. stirringthe mixture stirred for 18 h
2. stirringthe reaction stirred for 6 h
3. customThe mixture was quenched with water
4. customthe solvent removed in vacuo
5. additionWater was added
6. extractionthe mixture extracted with chloroform
7. dry with materialthe organic extracts dried (MgSO4)
8. filtrationfiltered
9. customevaporated in vacuo
10. customThe crude product was purified by preparative LC-MS