反应详情

To a mixture of the compound from step 1 (278 mg, 1.0 mmol) and K2CO3 (152 mg, 1.1 mmol) in DMF (5 mL) was added 3-bromopropyne (130 mg, 1.1 mmol) dropwise at rt. The reaction mixture was stirred at rt overnight and then partitioned between water and ethyl acetate. The organic payers were combined and washed with brine, dried over anhydrous Na2SO4 and evaporated under vacuum to give a brown oil. The crude product was purified by silica gel flash chromatography (30% ethyl acetate in hexane) to furnish the title compound (120 mg, 38%) as a light yellow solid; MS; m/z 317 (M+H).

1. custompartitioned between water and ethyl acetate
2. washwashed with brine
3. dry with materialdried over anhydrous Na2SO4
4. customevaporated under vacuum
5. customto give a brown oil
6. customThe crude product was purified by silica gel flash chromatography (30% ethyl acetate in hexane)