反应详情

Reaction was carried out in the same manner as in Reference example 15-(f) except for using 42.1 g (0.134 mol) of ethyl 2-methoxymethyl-1-(2-trimethylsilylethoxymethyl)-1H-pyrrol-3-carboxylate obtained in Reference example 15-(d) in place of ethyl 5-bromo-2-methoxymethyl-1-(2-trimethylsilylethoxymethyl)-1H-pyrrol-3-carboxylate. After completion of the reaction, 45 g of Celite and 200 ml of toluene were added to the reaction suspension, the mixture was stirred at room temperature for 30 minutes, and insoluble material was removed by filtration. The organic layer obtained by separating the filtrate was washed successively with a saturated aqueous solution of sodium hydrogencarbonate and then with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=9:1→7:3 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 37.7 g of the title compound as a colorless oil. (Yield: 95%)

1. customReaction
2. additionwere added to the reaction suspension
3. custominsoluble material was removed by filtration
4. customThe organic layer obtained
5. customby separating the filtrate
6. washwas washed successively with a saturated aqueous solution of sodium hydrogencarbonate
7. dry with materialwith a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. additionthe fractions containing the desired compound
10. concentrationwere concentrated under reduced pressure