反应详情

温度

90 °C

To a solution of 4-(cyclohexylamino)-8-(3-iodobenzyl)-1-pent-4-en-1-yl-1,3,8-triazaspiro[4.5]dec-3-en-2-one (920 mg, 1.72 mmol, intermediate I.1.d.1) and trans-bis(triphenylphosphine)palladium(II) chloride (121 mg, 0.17 mmol) in degassed DMF (11.5 mL) was added allyl tri-n-butyltin (0.61 mL, 1.98 mmol) in one portion. The reaction mixture was stirred at 90° C., sealed, for 16 h, diluted with EtOAc, washed with aqueous LiCl twice, dried over sodium sulfate, concentrated in vacuo and purified by flash chromatography (90 g silica gel, EtOAc) to give the desired product. LRMS (M+1)=449.

1. customsealed, for 16 h
2. washwashed with aqueous LiCl twice
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo
5. custompurified by flash chromatography (90 g silica gel, EtOAc)