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Step 34a To a dry flask is added methyl 1-methyl-1H-pyrrole-2-carboxylate (12.0 g, 86.4 mmol) and 150 mL of dry CH2Cl2, and the flask is wrapped in foil and purged with nitrogen. N-Bromosuccinimide (16.2 g, 90.7 mmol) is added in one portion and the mixture is stirred at rt for 0.5 h. The reaction mixture is washed with water (50 mL) and brine (50 mL), dried over MgSO4, filtered, and concentrated under reduced pressure. Fractional distillation gives 12.0 g of methyl 5-bromo-1-methyl-1H-pyrrole-2-carboxylate as a yellow oil (64% yield). MS for C7H8NO2Br (ESI) (M)+m/z 217.1.
With N-Bromosuccinimide; In chloroform; at 0 - 20℃;
To a solution of methyl 1 -methyl- lH-pyrrole-2-carboxylate_( 100 mg, 0.719 mmol) in CHCl3 (5 mL) at 0 C was added N-bromosuccinimide (128 mg, 0.719 mmol). The reaction was stirred at 0 C for 5 min. The reaction was allowed to warm to room temperature and stirred overnight. The reaction mixture was filtered and concentrated in vacuo. The residue was purified by preparative TLC (1000 muetaiota, hexanes/EtOAc (9:1)) to give methyl 5 -bromo- 1 -methyl- lH-pyrrole-2- carboxylate. NMR (500 MHz, CDCI3): 6 6.94 (d, J= 4.2 Hz, 1 H); 6.21 (d, J= 4.1 Hz, 1 H); 3.94 (s, 3 H); 3.82 (s, 3 H),
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