Imidazole → 1-Ethyl-2-(2-iodoethyl)benzene

Into a 50-mL round-bottom flask was placed ether (10 mL), CH3CN (5 mL) and 2-(2-ethylphenyl)ethan-1-ol (900 mg, 5.99 mmol, 1.00 equiv). Then imidazole (570 mg, 8.38 mmol, 1.40 equiv), PPh3 (2.20 g, 8.39 mmol, 1.40 equiv) and I2 (1.98 g, 7.80 mmol, 1.30 equiv) were added at 0° C. The resulting solution was stirred for 6 h at room temperature. The reaction was then quenched by the addition of 10 mL of saturated Na2SO3 solution. The resulting solution was extracted with 3×50 mL of ethyl acetate and the organic layers combined, dried over Na2SO4 and concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:20). Purification afforded 1.16 g (74%) of 1-ethyl-2-(2-iodoethyl)benzene as a colorless oil.

1. customInto a 50-mL round-bottom flask was placed
2. customThe reaction was then quenched by the addition of 10 mL of saturated Na2SO3 solution
3. extractionThe resulting solution was extracted with 3×50 mL of ethyl acetate
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under vacuum
6. customPurification

ORDレコード

ord-7202c06930704a939fa6991a4c43ed63

出典データセット

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08969557B2