반응 #553512

반응 방정식

magnesium

trimethylgermyl chloride

2-(3-bromophenyl)-2-methyl-1,3-dioxolane

→

pale yellow crystals

수율 103.7%

2-(3-Trimethylgermylphenyl)-2-methyl-1,3-dioxolane

수율 103.7%

용매

—

petroleum ether

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGwith stirring
2. 2
   온도The mixture was refluxed for 2.5 hr
3. 3
   workup.STIRRINGand stirred at room temperature overnight
4. 4
   여과the insoluble substance was filtered off
5. 5
   기타The filtrate was evaporated

실험 절차

A mixture of 81 mg (3.33 mmol) of magnesium and 574 mg (3.75 mmol) of trimethylgermyl chloride was stirred at 40°-50° C. in an atmosphere of argon. To the mixture was added a solution of 729 mg (3.00 mmol) of 2-(3-bromophenyl)-2-methyl-1,3-dioxolane in 10 ml of tetrahydrofuran with stirring. The mixture was refluxed for 2.5 hr. and stirred at room temperature overnight. To the reaction mixture was added petroleum ether and the insoluble substance was filtered off. The filtrate was evaporated to give 874 mg of pale yellow crystals, which were purified by column chromatography on silica gel [eluent: methylene chloride-n-hexane (1:1)] to give 657 mg of white cubes, m.p. 62.5°-63.5° C. (yield 78%).

출처