반응 #71035

반응 방정식

Na2CO3

N2

1-(3-bromo-phenyl)-ethanone

ethylene glycol

trimethylorthoformate

→

title compound

2-(3-Bromo-phenyl)-2-methyl-[1,3]dioxolane

반응 조건

후처리

1. 1
   추출the mixture was extracted twice with ether
2. 2
   건조the combined organic extracts were dried over Na2SO4
3. 3
   여과filtered
4. 4
   기타the solvent was removed under reduced pressure
5. 5
   기타Purification of the residue by FC (20:1 hept-EA)

실험 절차

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 1-(3-bromo-phenyl)-ethanone (1360 mg, 6.83 mmol) in ethylene glycol (8.00 mL, 143.46 mmol) was treated with trimethylorthoformate (1.50 mL, 13.68 mmol) followed by LiBF4 (131 mg, 1.37 mmol). The reaction mixture was heated at 95° C. for 15 h. Sat. aq. Na2CO3 was added and the mixture was extracted twice with ether and the combined organic extracts were dried over Na2SO4, filtered, and the solvent was removed under reduced pressure. Purification of the residue by FC (20:1 hept-EA) gave the title compound as a pale yellow oil: TLC:rf (10:1 hept-EA)=0.34. LC-MS-conditions 02: tR=1.01 min.

출처