反応 #82522

反応方程式

2-amino-4-hydroxy-6-methyl-5-[3-(2,5-dichlorophenyl)-2-butenyl]pyrimidine

phosphorus oxychloride

phosphorus pentachloride

→

2-amino-4-chloro-6-methyl-5-[3-(2,5-dichlorophenyl)-2-butenyl]pyrimidine

収率 97.3%

反応条件

後処理

1. 1
   温度at reflux for about 18 hours
2. 2
   ろ過the resultant solid is collected by filtration
3. 3
   workup.DISSOLUTIONThe solid is dissolved in methylene chloride
4. 4
   乾燥the solution is dried with magnesium sulfate
5. 5
   ろ過The mixture is filtered
6. 6
   濃縮the filtrate is concentrated under reduced pressure

実験手順

Under a nitrogen atmosphere, a stirred solution of 2.0 grams (0.006 mole) of 2-amino-4-hydroxy-6-methyl-5-[3-(2,5-dichlorophenyl)-2-butenyl]pyrimidine, 16.5 grams (0.107 mole) of phosphorus oxychloride, and 1.5 grams (0.007 mole) of phosphorus pentachloride is heated at reflux for about 18 hours. After this time the reaction mixture is slowly pipetted into wet ice during a 20 minute period. The mixture is then stirred until the ice melted, and the resultant solid is collected by filtration. The solid is dissolved in methylene chloride, and the solution is dried with magnesium sulfate. The mixture is filtered and the filtrate is concentrated under reduced pressure, yielding 2.0 grams of 2-amino-4-chloro-6-methyl-5-[3-(2,5-dichlorophenyl)-2-butenyl]pyrimidine; mp 97°-100° C. The NMR spectrum is consistent with the proposed structure.

出典