تفاعل #71035

معادلة التفاعل

Na2CO3

N2

1-(3-bromo-phenyl)-ethanone

ethylene glycol

trimethylorthoformate

→

title compound

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

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe mixture was extracted twice with ether
2. 2
   تجفيفthe combined organic extracts were dried over Na2SO4
3. 3
   ترشيحfiltered
4. 4
   أخرىthe solvent was removed under reduced pressure
5. 5
   أخرىPurification of the residue by FC (20:1 hept-EA)

الإجراء التجريبي

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.

المصدر