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ChemicalBook CAS DataBase List 2,4-DIBROMOANISOLE

2,4-DIBROMOANISOLE synthesis

15synthesis methods
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Yield: 98.8%

Reaction Conditions:

Stage #1:2,4-dibromophenol with potassium carbonate in acetonitrile for 0.166667 h;
Stage #2:methyl iodide in acetonitrile at 0 - 60; for 12 h;

Steps:

F.i
Preparation F 4-f3-bromopropoxy)isophthalonitrile(i) 2.4-Dibromo-l-methoxybenzeneK2CO3 (34.5 g, 0.243 mol) was added to a solution of 2,4-dinitrophenol (25 g, 0.009 mol) in acetonitrile (250 mL) and stirred for 10 minutes. The reaction mixture was cooled to O0C, methyl iodide (15 mL, 0.240 mol) was added and the reaction mixture was stirred at 6O0C for 12 h under a nitrogen atmosphere. The reaction mixture was cooled to RT and filtered through a Celite bed. The filtrate was concentrated under reduced pressure to afford 2,4-dibromo-l- EPO methoxybenzene (26 g, 98.8%) as brown solid product. This was employed directly in the next step without further purification.

References:

ASTRAZENECA AB WO2006/135316, 2006, A1 Location in patent:Page/Page column 61-62

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