반응 #3005

반응 방정식

potassium carbonate

benzyl chloride

4-hydroxy-6-methyl-2H-pyran-2-one

18-crown-6

→

4-Benzyloxy-6-methyl-2H-pyran-2-one

용매

dimethyl-formamide

반응 조건

후처리

1. 1
   여과filtered
2. 2
   세척the residue was washed well with ethyl acetate
3. 3
   기타The combined filtrates were extensively evaporated in a vacuum
4. 4
   workup.ADDITIONsubsequently poured onto ice water
5. 5
   기타The aspirated precipitate was recrystallized from t-butylmethyl ether
6. 6
   기타after drying

실험 절차

124.4 g (0.900 mol) potassium carbonate and 63 ml (0.547 mol) benzyl chloride were added in succession to a solution of 56.7 g (0.450 mol) 4-hydroxy-6-methyl-2H-pyran-2-one and 1.0 g (0.004 mol) 18-crown-6 in 900 ml anhydrous dimethyl-formamide. It was stirred vigorously for 4.5 hours at an internal temperature of 70°-75° C. It was suction filtered and the residue was washed well with ethyl acetate. The combined filtrates were extensively evaporated in a vacuum and subsequently poured onto ice water. The aspirated precipitate was recrystallized from t-butylmethyl ether after drying. 69.0 g (71%) V, melting point 92°-93° C.

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