반응 #367984

반응 방정식

2-amino-4-methoxy-6-methylpyrimidine

2-methoxycarbonylbenzenesulfonyl isocyanate

→

product

수율 21.1%

N-[(4-Methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamide

수율 21.1%

용매

methylene chloride

반응 조건

후처리

1. 1
   여과the foregoing mixture was filtered
2. 2
   기타to remove unreacted amine
3. 3
   기타the filtrate evaporated at temperatures up to 40°
4. 4
   workup.STIRRINGThe resultant residue was stirred in 25 ml of water
5. 5
   workup.ADDITIONthe pH adjusted to 10 by the addition of 50% sodium hydroxide
6. 6
   여과the solution filtered
7. 7
   기타precipitation of the desired product which
8. 8
   기타was removed by filtration
9. 9
   기타dried

실험 절차

To a stirred suspension of 1.4 g of 2-amino-4-methoxy-6-methylpyrimidine in 30 ml of anhydrous methylene chloride was added at ambient temperature 2.4 g of 2-methoxycarbonylbenzenesulfonyl isocyanate. After stirring for 16 hours, the foregoing mixture was filtered to remove unreacted amine, and the filtrate evaporated at temperatures up to 40° and reduced pressure. The resultant residue was stirred in 25 ml of water, the pH adjusted to 10 by the addition of 50% sodium hydroxide and the solution filtered. Acidification of the filtrate to pH 3 with hydrochloric acid caused precipitation of the desired product which was removed by filtration and dried to yield 0.8 g of product melting at 173°-179°. It showed infrared absorption peaks at 1720, 1680, 1630 and 1550 cm-1, consistent for N-[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]-2-methoxycarbonylbenzenesulfonamide.

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