反应详情

To a mixture of 5-benzyloxy-2-iodo-4-methoxybenzoic acid (reference example 5-2) (1.92 g), piperidine (0.74 mL) and N,N-dimethylforamide (12 mL) was added 1-hydroxybenzotriazole (676 mg) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (1.44 g) at room temperature. The mixture was stirred at room temperature for 6 hours. After addition of ethyl acetate, the mixture was poured into 2 mol/L hydrochloric acid. The organic layer was washed with water, an aqueous solution of sodium bicarbonate, and brine successively, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The mixture of the residue, aminopropylsilicagel and dichloromethane was stirred for 30 minutes. Insoluble materials were removed by filtration. The filtrate was concentrated under reduced pressure to give the title compound (2.13 g).

1. washThe organic layer was washed with water
2. dry with materialan aqueous solution of sodium bicarbonate, and brine successively, dried over anhydrous magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. additionThe mixture of the residue
5. stirringaminopropylsilicagel and dichloromethane was stirred for 30 minutes
6. customInsoluble materials were removed by filtration
7. concentrationThe filtrate was concentrated under reduced pressure