反应 #4005

反应方程式

sodium

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

sodium methoxide

→

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

溶剂

methanol

methanol

反应条件

后处理

1. 1
   其他prepared
2. 2
   workup.ADDITIONwas added dropwise, over 30 minutes at ambient temperature
3. 3
   其他had been consumed
4. 4
   其他The product was precipitated by the addition of water
5. 5
   过滤filtered
6. 6
   其他dried
7. 7
   其他The solid obtained
8. 8
   其他was purified by chromatography on silica
9. 9
   其他Final purification
10. 10
    其他was effected by recrystallisation from carbon tetrachloride

实验过程

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.

来源