1-Iodo-4-isopropyl-2-methoxybenzene synthesis

7synthesis methods

Product Name:1-Iodo-4-isopropyl-2-methoxybenzene
CAS Number:1240304-64-6
Molecular formula:C10H13IO
Molecular Weight:276.11

1017608-23-9 Synthesis

1017608-23-9
7 suppliers
inquiry

74-88-4
343 suppliers
$15.00/10g

1240304-64-6
19 suppliers
inquiry

Yield:1240304-64-6 85%

Reaction Conditions:

with potassium carbonate in acetonitrile at 40; for 3.5 h;

Steps:

1.2 Reference Example 1-2 Compound (B2)

Reference Example 1-2 Compound (B2) [0121] [0122] Methyl iodide (9.8 mL, 0.156 mol) was added to an acetonitrile suspension (200 mL) of the compound (B1) (27.4 g, 0.104 mol) and potassium carbonate (21.7 g, 0.156 mol), and the mixture was stirred for 2.5 hours at 40° C. Methyl iodide (3.5 mL, 0.052 mol) was further added, and the mixture was stirred for 1 hour at the same temperature. Insolubles were filtered out, and the filtrate was diluted with ethyl acetate. The organic layer was washed with water, a 10% aqueous solution of sodium thiosulfate, and brine, and dried over anhydrous magnesium sulfate. The desiccant was filtered out, and then the solvent was distilled off under reduced pressure. The resulting residue was purified by neutral silica gel column chromatography (hexane→hexane:ethyl acetate=95:5) to obtain a light yellow oily compound (B2) (24.5 g, 85%). [0123] ¹H NMR (300 MHz, CHLOROFORM-d) δ ppm 1.24 (d, J=6.84 Hz, 6H) 2.87 (quin, J=6.92 Hz, 1H) 3.88 (s, 3H) 6.58-6.65 (m, 1H) 6.70 (d, J=1.87 Hz, 1H) 7.65 (d, J=8.08 Hz, 1H). MS ESI/APCI Dual posi: 277[M+H]⁺.

References:

US2013/144050,2013,A1 Location in patent:Paragraph 0121; 0122; 0123