Methyl iodide → 3-Bromo-2-methyl-1-benzothiophene

온도

-78 °C

1.06 g of 3-Bromo-benzo[b]thiophene (5.0 mmol) is dissolved in 10 ml of dry tetrahedrofuran and cooled to −78° C. and 3.67 ml of lithium diisopropylamine 1.5M in cyclohexane (5.5 mmol) is added slowly and stirred at −78° C. for 15 min. 0.35 ml of Methyl iodide (5.6 mmol) is added and the reaction mixture is stirred at room temperature for 1 h, sat. NH4Cl is added, and the mixture is extracted with CH2Cl2, dried over Na2SO4 and evaporated. The crude product is applied onto a silica-gel chromatography column (Hexane:AcOEt=10:1) to give the title compound. 835 mg (74%). 1H-NMR (CDCl3): 7.76 (t, 2H, J=7.7 Hz), 7.46 (t, 1H, J=7.7 Hz), 7.37 (t, 1H, J=7.7 Hz), 2.60 (s, 3H)

1. stirringthe reaction mixture is stirred at room temperature for 1 h
2. extractionthe mixture is extracted with CH2Cl2
3. dry with materialdried over Na2SO4
4. customevaporated

ORD 기록

ord-c2822ee6fd1a4030ba0a2bdd663f0cd9

출처 데이터셋

uspto-grants-2009_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07557103B2