반응 #4005

반응 방정식

sodium

2-amino-4-chloro-6-(2,2-dichlorovinyl)pyrimidine

sodium methoxide

→

2-amino-4-(2,2-dichlorovinyl)-6-methoxypyrimidine

용매

methanol

methanol

반응 조건

후처리

1. 1
   기타prepared
2. 2
   workup.ADDITIONwas added dropwise, over 30 minutes at ambient temperature
3. 3
   기타had been consumed
4. 4
   기타The product was precipitated by the addition of water
5. 5
   여과filtered
6. 6
   기타dried
7. 7
   기타The solid obtained
8. 8
   기타was purified by chromatography on silica
9. 9
   기타Final purification
10. 10
    기타was effected by recrystallisation from carbon tetrachloride

실험 절차

22.0 Parts of 2-amino-4-chloro-6-(2,2-dichlorovinyl)pyrimidine was dissolved in 500 parts of dry methanol and stirred whilst a solution of sodium methoxide, prepared by dissolving 4.6 parts of sodium in 200 parts of dry methanol, was added dropwise, over 30 minutes at ambient temperature. The resulting solution was stirred for 4 hours by which time all the starting material had been consumed. The product was precipitated by the addition of water, filtered and dried. The solid obtained was purified by chromatography on silica using diethyl ether as eluent. Final purification was effected by recrystallisation from carbon tetrachloride to give 2-amino-4-(2,2-dichlorovinyl)-6-methoxypyrimidine m.p. 90°-91° C.

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