反应详情

To a mixture of 4-iodo-benzoyl chloride (75 g) in 500 mL CH2Cl2 was added a mixture of Et3N (50 mL) and Et2NH (100 mL) at 0° C. After the addition, the resulting reaction mixture was warmed up to room temperature in 1 hr and was then washed with saturated ammonium chloride. The organic extract was dried (Na2SO4), filtered and concentrated. Residue was recrystallized from hot hexanes to give 80 g of INTERMEDIATE 5.

1. additionwas added
2. additionAfter the addition
3. customthe resulting reaction mixture
4. washwas then washed with saturated ammonium chloride
5. extractionThe organic extract
6. dry with materialwas dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customResidue was recrystallized from hot hexanes