反应详情

A mixture of N-{[(2S)-8-fluoro-2,3-dihydro-1,4-benzodioxin-2-yl]methyl}ethanamine (1.95 g, 9.2 mmol), K2CO3 (2.55 g, 18.5 mmol), benzylbromide (1.3 ml, 11.1 mmol), a spatula of NaI (<5 mg) and acetonitrile was heated under microwave radiation at 120° C. for 20 min. The solution was filtered and evaporated, Na2CO3 (10%) was added and the solution was extracted with EtOAc. The combined organic phases were dried (Na2SO4) and evaporated to dryness. Purification on flash column chromatography (isooctane/EtOAc) yielded 2.3 g of the title compound. MS m/z (rel. intensity, 70 eV) 149 (10), 148 (86), 92 (8), 91 (bp), 65 (7).

1. filtrationThe solution was filtered
2. customevaporated
3. additionNa2CO3 (10%) was added
4. extractionthe solution was extracted with EtOAc
5. dry with materialThe combined organic phases were dried (Na2SO4)
6. customevaporated to dryness
7. customPurification on flash column chromatography (isooctane/EtOAc)