반응 #67106

반응 방정식

5-bromo-2-(methyloxy)-3-pyridinamine

2,4-difluorobenzenesulfonyl chloride

→

desired material

수율 5.9%

N-[5-Bromo-2-(methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide

수율 5.9%

용매

pyridine

반응 조건

후처리

1. 1
   기타(reaction became heterogeneous)
2. 2
   기타The ice bath was removed
3. 3
   기타Most of the pyridine was removed in vacuo
4. 4
   workup.ADDITIONthe residue diluted with water (500 mL)
5. 5
   여과The solids were filtered off
6. 6
   세척washed with copious amounts of water
7. 7
   기타to give 21 g of crude desired product
8. 8
   여과was filtered
9. 9
   세척washed with water

실험 절차

To a cooled (0° C.) solution of 5-bromo-2-(methyloxy)-3-pyridinamine (13.7 g, 67.5 mmol) in pyridine (200 ml) was added slowly 2,4-difluorobenzenesulfonyl chloride (14.37 g, 67.6 mmol) over 15 min (reaction became heterogeneous). The ice bath was removed and the reaction was stirred at ambient temperature for 16 h. Most of the pyridine was removed in vacuo and the residue diluted with water (500 mL). The solids were filtered off and washed with copious amounts of water to give 21 g of crude desired product. More solid appeared in the mother liquor and was filtered and washed with water to give an additional 1.5 g of desired material. The two batches were combined, triturated with 70 ml of methylene chloride, and dried in a vacuum oven at 50° C. to give the title compound (15 g).

출처