반응 #213940

반응 방정식

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

acetic anhydride

→

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

수율 66.0%

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 2 hours
3. 3
   workup.DISTILLATIONThe mixture was then distilled at atmospheric pressure over 2 hours
4. 4
   workup.ADDITIONfresh acetic anhydride being added
5. 5
   온도to maintain the original volume
6. 6
   workup.DISTILLATIONThe mixture was then distilled at atmospheric pressure so that the final volume
7. 7
   workup.ADDITIONwas then added
8. 8
   기타The white solid which precipitated
9. 9
   세척was washed with ether (2×30 ml.) and air
10. 10
    기타dried

실험 절차

A mixture of 3-(3-trifluoromethylphenyl)-6-n-butylaminotetrahydro-1,3,5-triazine-2,4-dione (4.0 g.) and acetic anhydride (40 ml.) was heated under reflux for 2 hours. The mixture was then distilled at atmospheric pressure over 2 hours, fresh acetic anhydride being added to maintain the original volume. The mixture was then distilled at atmospheric pressure so that the final volume was about 10 ml. Ether (60 ml.) and petroleum ether (b.p. 40°-60° C.) [hereinafter referred to as "40-60 petrol"] (20 ml.) was then added. The white solid which precipitated was washed with ether (2×30 ml.) and air dried to give 3-(3-trifluoromethylphenyl)-6-[(N-acetyl)-n-butylamino]-tetrahydro-1,3,5-triazine-2,4-dione (3.7 g., 66%), m.p. 146°-148° C.

출처