ChemicalBook CAS DataBase List 1-Iodo-3,5-dimethylbenzene

1-Iodo-3,5-dimethylbenzene synthesis

11synthesis methods

Product Name:1-Iodo-3,5-dimethylbenzene
CAS Number:22445-41-6
Molecular formula:C8H9I
Molecular Weight:232.06

556-96-7
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22445-41-6
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$5.00/5g

Yield:22445-41-6 78 - 98 %Chromat.

Reaction Conditions:

with trans-N,N'-dimethyl-1,2-cyclohexyldiamine;sodium iodide;copper(l) iodide in toluene at 110; for 23 h;

Steps:

9; 10 Example 9; Preparation of [5-IODO-M-XYLENE USING] Various Solvents
A Schlenk tube was charged with Cul (9.6 mg, 0.0504 mmol, 5.0 mol%), sodium iodide (fine powder, dried, 300 mg, 2.00 mmol), evacuated and backfilled with argon. [TRANS-N, N'-DIMETHYL-1,] 2-cyclohexanediamine (16 [ILL,] 0.10 mmol, 10 [MOL%),] 5-bromo-m- xylene [(136 GEL,] 1.00 mmol), and solvent (1.0 mL) were added under argon. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at [110 °C] for 23 h. The resulting suspension was allowed to reach room temperature. Ethyl acetate (2 mL) and dodecane (internal GC standard, 230 μL) were added to the reaction mixture. A 50 μL sample of the supernatant solution was diluted with ethyl acetate (1 mL) and analyzed by GC. The results are tabulated below.; A Schlenk tube was charged with CuI, sodium iodide (fine powder, dried, 300 mg, 2.00 mmol), evacuated and backfilled with argon. [N, N'-DIMETHYLETHYLENEDIAMINE,] 5- [BROMO-M-XYLENE] (136 [UL,] 1.00 mmol), and toluene (1.0 mL) were added under argon. The Schlenk tube was sealed with a Teflon valve and the reaction mixture was stirred at [110 °C] for 22 h. The resulting suspension was allowed to reach room temperature. Ethyl acetate (2 mL) and dodecane (internal GC standard, [230 GEL)] were added to the reaction mixture. A 50 pL sample of the supernatant solution was diluted with ethyl acetate (1 mL) and analyzed by GC. The results are tabulated below.

References:

MASSACHUSETTS INSTITUTE OF TECHNOLOGY WO2004/13094, 2004, A2 Location in patent:Page 45

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172975-69-8 Synthesis