반응 #323704

반응 방정식

2-amino-4,6-dichloropyrimidine

NaOCH3

→

product

수율 58.9%

2-Amino-4-chloro-6-methoxypyrimidine

수율 58.9%

용매

CH3OH

반응 조건

후처리

1. 1
   온도The mixture was cooled to 10° with an ice bath
2. 2
   온도while maintaining the temperature
3. 3
   온도heated
4. 4
   온도to reflux for two hours
5. 5
   온도to cool to ambient temperature
6. 6
   여과A yellow solid was filtered
7. 7
   기타recrystallized from butyl chloride
8. 8
   기타The resulting solid was chromatographed on a dry column of silica
9. 9
   세척eluted with 40% EtOAc-hexane
10. 10
    기타The resulting yellow solid was further purified by recrystallization from butyl chloride

실험 절차

16.4 g 2-amino-4,6-dichloropyrimidine (purchased from Aldrich Chemical Co., Milwaukee, WI 53201) was added to 200 ml of CH3OH. The mixture was cooled to 10° with an ice bath and 5.4 g of NaOCH3 was added in portions while maintaining the temperature. The reaction mixture was allowed to warm to ambient temperature and then heated to reflux for two hours. The reaction mixture was then allowed to cool to ambient temperature and it was stirred overnight. A yellow solid was filtered and recrystallized from butyl chloride. The resulting solid was chromatographed on a dry column of silica, and eluted with 40% EtOAc-hexane. The resulting yellow solid was further purified by recrystallization from butyl chloride. 9.4 g of product with m.p. 163°-166° was obtained.

출처