تفاعل #3005
ord-9faac40bc60f4f9481fb3e21ace77f7b
معادلة التفاعل
الكواشف
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المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1ترشيحfiltered
- 2غسيلthe residue was washed well with ethyl acetate
- 3أخرىThe combined filtrates were extensively evaporated in a vacuum
- 4workup.ADDITIONsubsequently poured onto ice water
- 5أخرىThe aspirated precipitate was recrystallized from t-butylmethyl ether
- 6أخرىafter drying
الإجراء التجريبي
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.