反应详情

To a solution of 4-iodophenol (30 mmol) in CH2Cl2 (100 mL) was added N-methyl-N-phenylcarbamoyl chloride (27 mmol) and diisopropylethylamine (60 mmol) at room temperature. The reaction mixture was stirred for 16 hours at rt, added CH2Cl2 (20 mL) and washed with aqueous citric acid (5%), aqueous Na2CO3 and brine. The organic phase was dried (MgSO4) and evaporated to give the crude product which was purified by FC (Quad flash 40 EtOAc-Heptane) to give 6.55 g (69%) of the title compound as light brown crystals.

1. washwashed with aqueous citric acid (5%), aqueous Na2CO3 and brine
2. dry with materialThe organic phase was dried (MgSO4)
3. customevaporated
4. customto give the crude product which
5. customwas purified by FC (Quad flash 40 EtOAc-Heptane)