反应详情

To an ice cold solution of 1.60 g (0.04 mol) of NaOH in 45 ml of water is added 9.64 g (0.04 mol) of 5-cyano-1-(2,6-dimethylphenyl)uracil, obtained as in Example 1. After dissolution, 50 ml of ice cold dichloromethane is added, followed by a solution of 9.36 g (0.04 mol) of 1,1,2,2-tetrachloroethanesulphenyl chloride (prepared by the method of U.S. Pat. No. 3,395,180) in 15 ml. of dichloromethane. The mixture is stirred for 30 min at 4°. The aqueous layer is separated and discarded. The dichloromethane solution is dried and stripped at aspirator pressure. The unreacted sulphenyl chloride is then removed by trituration with pentane/dichloromethane (4:1). The resultant crude product is purified by slurrying at 30° in 60 ml of ethanol-free chloroform, allowed to cool to RT and filtered. To the filtrate is added hexane to the cloud point, and the mixture is then filtered to yield 5-cyano-1-(2,6-dimethylphenyl)-3-(1,1,2,2-tetrachloroethanesulphenyl)uracil, m.p. 180°-183°.

1. customobtained as in Example 1
2. additionis added
3. customprepared by the method of U.S
4. customThe aqueous layer is separated
5. dry with materialThe dichloromethane solution is dried
6. customThe unreacted sulphenyl chloride is then removed by trituration with pentane/dichloromethane (4:1)
7. customThe resultant crude product is purified
8. customby slurrying at 30° in 60 ml of ethanol-free chloroform
9. filtrationfiltered
10. additionTo the filtrate is added hexane to the cloud point
11. filtrationthe mixture is then filtered