반응 #213942

반응 방정식

n-Butylamine

3-(3-trifluoromethylphenyl)-6-methylthio-tetrahydro-1,3,5-triazine-2,4-dione

→

3-(3-trifluoromethylphenyl)-6-n-butylamino-tetrahydro-1,3,5-triazine-2,4-dione

수율 95.0%

용매

acetic acid

acetic acid

반응 조건

후처리

1. 1
   기타The mixture obtained
2. 2
   기타(The liberated methylmercaptan was absorbed into a trap
3. 3
   workup.ADDITIONcontaining an excess of aqueous sodium hydroxide and sodium hypochlorite
4. 4
   온도) The reaction mixture was cooled to room temperature
5. 5
   workup.ADDITIONwater (75 ml.) was added
6. 6
   기타the white solid which formed
7. 7
   기타was separated by filtration
8. 8
   세척washed with water (3×150 ml.)
9. 9
   건조dried (over phosphorus pentoxide)

실험 절차

n-Butylamine (3.92 ml.) was added during 15 minutes to stirred acetic acid (2.4 ml.). After 30 minutes at room temperature, 3-(3-trifluoromethylphenyl)-6-methylthio-tetrahydro-1,3,5-triazine-2,4-dione (6.1 g.) was added to the acetic acid solution. The mixture obtained was then heated at 145° C., for 4 hours. (The liberated methylmercaptan was absorbed into a trap containing an excess of aqueous sodium hydroxide and sodium hypochlorite.) The reaction mixture was cooled to room temperature and then water (75 ml.) was added. The mixture was then stirred for 15 minutes and the white solid which formed was separated by filtration, washed with water (3×150 ml.), and dried (over phosphorus pentoxide) to give 3-(3-trifluoromethylphenyl)-6-n-butylamino-tetrahydro-1,3,5-triazine-2,4-dione (6.0 g., 95%), m.p. 245°-247° C.

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