反应详情

To a suspension of 4-chloro-1H-pyrrolo[2,3-b]pyridine-5-carbaldehyde (2.00 g, 11.1 mmol, Adesis) in DMF (30 mL) was added NaH (60% dispersion in mineral oil, 0.500 g, 12.5 mmol) forming a yellow solution. The reaction mixture was stirred at ambient temperature for about 30 min then 4-methylbenzene-1-sulfonyl chloride (2.40 g, 12.6 mmol) was added. The reaction mixture was stirred at ambient temperature for about 30 min and poured into ice water (about 50 mL). The solid was collected via vacuum filtration, while washing with water (about 15 mL), and dried in a vacuum oven to give 4-chloro-1-tosyl-1H-pyrrolo[2,3-b]pyridine-5-carbaldehyde (3.22 g, 87%) as an off white solid: LC/MS (Table 1, Method b) Rt=2.56 min; MS m/z: 335 (M+H)+.

1. customforming a yellow solution
2. stirringThe reaction mixture was stirred at ambient temperature for about 30 min
3. filtrationThe solid was collected via vacuum filtration
4. washwhile washing with water (about 15 mL)
5. customdried in a vacuum oven