METHYL 5-IODO-2-METHOXY-4-METHYLBENZOATE synthesis
- Product Name:METHYL 5-IODO-2-METHOXY-4-METHYLBENZOATE
- CAS Number:914225-32-4
- Molecular formula:C10H11IO3
- Molecular Weight:306.1
81245-24-1
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Yield:914225-32-4 94.2 %
Reaction Conditions:
with iodine;silver trifluoromethanesulfonate in methanol at 25;
Steps:
In methanol (15 mL) solution with compound INT-13b (1.0 g, 5.55 mmol) dissolved silver triflate (1.57 g, 6.10 mmol) and iodine (1.55 g, 6.10 mmol) were added. The reaction solution was stirred for 2 hours at 25°C, subsequently was filtered, and the filtrate was diluted with ethyl acetate (50 mL), and was wased with sodium sulfite aqueous solution (5% w/w, 50 mL) and saturated salt solution (100 mL), dried with anhydrous sodium sulfate, filtered, and concentrated to obtain orange solid INT-13 (1.6 g, yield: 94.2%). 1H NMR (500 MHz, Chloroform-d) δ 8.20 (s, 1H), 6.86 (s, 1H), 3.88 (s, 3H), 3.87 (s, 3H), 2.45 (s, 3H); MS (ESI): m/z 306.9 (M+H)+.
References:
EP4083032,2022,A1 Location in patent:Paragraph 0188; 0191
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4670-56-8
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