Реакция #1435698

Уравнение реакции

3-Methyl-1-phenylpyrazol-5-one

calcium hydroxide

tert-butylacetyl chloride

→

4-tert-Butyl-3-methyl-1-phenylpyrazol-5-one

Растворители

HCl

Условия реакции

Обработка

1. 1
   Другоеequipped with a stirrer
2. 2
   Температураreflux condenser
3. 3
   ДругоеDry
4. 4
   workup.DISTILLATIONdistilled dioxane (40 ml)
5. 5
   workup.ADDITIONwas added
6. 6
   workup.ADDITIONwas added
7. 7
   ТемператураThe mixture was heated
8. 8
   Температураto reflux for 4 hours
9. 9
   ДругоеA light brown precipitate formed immediately
10. 10
    Фильтрацияwhich was filtered off under suction
11. 11
    ПромывкаThe product was washed with water
12. 12
    Другоеdried under vacuum at 50° C
13. 13
    ДругоеThe product was recrystallised from methanol
14. 14
    Другоеto give an off-white crystalline solid, m.p 85–86° C.

Методика

3-Methyl-1-phenylpyrazol-5-one (5 g; 0.029 mole) was placed in a flask equipped with a stirrer and reflux condenser. Dry and distilled dioxane (40 ml) was added by warming and to the clear solution calcium hydroxide (6.4 g; 0.086 mole) was added followed by drop wise addition of tert-butylacetyl chloride (4.8 ml; 0.034 mole). The mixture was heated to reflux for 4 hours and then poured into 2M HCl (200 ml) to decompose the calcium complex. A light brown precipitate formed immediately, which was filtered off under suction after refrigerating overnight. The product was washed with water and dried under vacuum at 50° C. The product was recrystallised from methanol to give an off-white crystalline solid, m.p 85–86° C.; 6.8 g (82%).

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