تفاعل #1370

معادلة التفاعل

2-methyl-3,4,6-trifluorobenzoyl chloride

sulfuric acid

magnesium

diethyl malonate

→

diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate

المذيبات

toluene

water

ethanol

toluene

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONis added dropwise below 60° C
2. 2
   درجة الحرارةthe reaction mixture is cooled to 0° C.
3. 3
   workup.ADDITIONis added dropwise
4. 4
   workup.STIRRINGAfter stirring for 30 minutes
5. 5
   workup.ADDITIONis added
6. 6
   استخلاصthe mixture is extracted with diethyl ether
7. 7
   تجفيفthe extract is dried over magnesium sulfate
8. 8
   تركيزconcentrated

الإجراء التجريبي

Separately, two drops of carbon tetrachloride are added to a solution of metallic magnesium (0.4 g) in absolute ethanol (0.9 ml). When the reaction starts, a mixture of diethyl malonate (2.6 ml), absolute ethanol (1.6 ml) and anhydrous toluene (6 ml) is added dropwise below 60° C. After stirring at 60° C. for 1 hour, the reaction mixture is cooled to 0° C. and thereto a solution of 2-methyl-3,4,6-trifluorobenzoyl chloride prepared above in toluene (5 ml) is added dropwise. After stirring for 30 minutes, a mixture of conc. sulfuric acid (0.4 ml) and water (6 ml) is added and the mixture is extracted with diethyl ether, and the extract is dried over magnesium sulfate and concentrated to give diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate (5.2 g).

المصدر