反应详情

Trimethoxymethane (1.18 ml, 10.78 mmol) was added to a solution of ethyl 5-methyl-1H-pyrrole-2-carboxylate (Intermediate 20) (0.5 g, 3.26 mmol) in TFA (2.5 ml) at 0° C. The reaction was stirred at that temperature for 10 mins then quenched with cold water (20 ml). The layers were separated and the aqueous layer was extracted with EtOAc. The combined organic extracts were dried over magnesium sulfate and concentrated to give yellow solid which was purified by flash chromatography (10% to 20% EtOAc in hexanes, 0.25 g).

1. customthen quenched with cold water (20 ml)
2. customThe layers were separated
3. extractionthe aqueous layer was extracted with EtOAc
4. dry with materialThe combined organic extracts were dried over magnesium sulfate
5. concentrationconcentrated
6. customto give yellow solid which
7. customwas purified by flash chromatography (10% to 20% EtOAc in hexanes, 0.25 g)