반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10]O)[CH3:2].N1C=CN=C1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[I:36]I>CC#N.CCOCC>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][I:36])[CH3:2]참가 물질
실험 절차
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.
후처리
- customInto a 50-mL round-bottom flask was placed
- customThe reaction was then quenched by the addition of 10 mL of saturated Na2SO3 solution
- extractionThe resulting solution was extracted with 3×50 mL of ethyl acetate
- dry with materialdried over Na2SO4
- concentrationconcentrated under vacuum
- customPurification
출처 및 근거
- ORD 기록
- ord-7202c06930704a939fa6991a4c43ed63
- 출처 데이터셋
- uspto-grants-2015_03
- 특허 번호
- US08969557B2
연결된 노트
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