반응 #486773

반응 방정식

1-Benzyl-1-(cyanoacetyl)-3-[3-(methylthio)phenyl]urea

sodium hydroxide

ethyl acetate

toluene

→

6-AMINO-3-BENZYL-1-[3-(METHYLTHIO)PHENYL]URACIL

용매

ethanol

water

반응 조건

후처리

1. 1
   workup.WAITto stand overnight at room temperature
2. 2
   여과The mixture was filtered
3. 3
   기타to remove a dark impurity
4. 4
   workup.ADDITIONthe filtrate carbon treated
5. 5
   기타This solution was then evaporated
6. 6
   기타to remove ethanol
7. 7
   workup.ADDITIONthen diluted with water
8. 8
   추출It was extracted with ethyl acetate (150 ml)
9. 9
   세척the extracts washed with water (2×75 ml)
10. 10
    기타then dried
11. 11
    기타evaporated
12. 12
    기타to give a foam
13. 13
    workup.WAITAfter standing for 1 h
14. 14
    기타the product had precipitated
15. 15
    여과It was filtered off
16. 16
    세척washed with 1:1 toluene/hexane (50 ml)
17. 17
    기타then dried to constant weight

실험 절차

1-Benzyl-1-(cyanoacetyl)-3-[3-(methylthio)phenyl]urea (14.9 g) was suspended in ethanol (150 ml) and to this was added a solution of sodium hydroxide (2.34 g) in water (30 ml). This was stirred for 1 h then allowed to stand overnight at room temperature. The mixture was filtered to remove a dark impurity and the filtrate carbon treated. This solution was then evaporated to remove ethanol then diluted with water. It was extracted with ethyl acetate (150 ml) and the extracts washed with water (2×75 ml) then dried and evaporated to give a foam. This was taken up in a 1:1 mixture of ethyl acetate and toluene (100 ml). After standing for 1 h the product had precipitated. It was filtered off and washed with 1:1 toluene/hexane (50 ml) then dried to constant weight. Yield=9.06 g.

출처