反应详情

温度

90 °C

A 50 ml two-neck round bottom flask was filled with argon gas and the solution of tetrakis(triphenyl phosphine)palladium(0) (123.7 mg, 0.107 mmol, 0.06 eq.) and lithium chloride (211.9 mg, 4.998 mmol, 2.8 eq.) in DMF was put into the flask. To the solution was added (4-amino-3-iodobenzyl) carbamic acid t-butyl ester (621.4 mg, 1.875 mmol, 1 eq.) and tributylvinyltin (782.5 mg, 2.678 mmol, 1.5 eq.). The mixture solution was heated to 90° C. to reflux for one night. After confirming the completion of the reaction with TLC, the reaction solution was extracted with methylenechloride, washed with water and brine, dried over Na2SO4, filtered and evaporated. The obtained liquid was column-chromatographed (n-hexane/ethyl acetate=3/1) to yield brown liquid.

1. additionA 50 ml two-neck round bottom flask was filled with argon gas
2. temperatureto reflux for one night
3. customthe completion of the reaction with TLC
4. extractionthe reaction solution was extracted with methylenechloride
5. washwashed with water and brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. customevaporated
9. customThe obtained liquid was column-chromatographed (n-hexane/ethyl acetate=3/1)
10. customto yield brown liquid