反应详情

温度

-5 °C

Ethyl 5-methyl-1H-pyrrole-2-carboxylate (Intermediate 20, 12.3 g, 0.803 mmol) was dissolved in anhydrous DCM and cooled to −5° C. N-bromosuccinimide (14.23 g; 0.0803 mmol) was added and the reaction stirred for 10 min and then poured into ice-cold 2 N sodium hydroxide (500 ml). The brown solution was extracted with EtOAc (2×150 ml), the combined organic extracts were washed with water, brine and dried over Na2SO4, then concentrated in vacuo to give a brown solid which was dried under vacuum. (16.5 g).

1. extractionThe brown solution was extracted with EtOAc (2×150 ml)
2. washthe combined organic extracts were washed with water, brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. customto give a brown solid which
6. customwas dried under vacuum