Methyl 3-fluoro-5-iodo-4-Methylbenzoate synthesis
- Product Name:Methyl 3-fluoro-5-iodo-4-Methylbenzoate
- CAS Number:861905-21-7
- Molecular formula:C9H8FIO2
- Molecular Weight:294.06
67-56-1
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861905-94-4
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861905-21-7
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Yield:861905-21-7 100%
Reaction Conditions:
with sulfuric acid in water at 20 - 50; for 15 h;Product distribution / selectivity;
Steps:
1.3
Preparation of methyl 3-fluoro-5-iodo-4-methylbenzoate; 3-Fluoro-5-iodo-4-methylbenzoic acid (1 eqv) was dissolved in methanol (6.6 vol) and treated with 98% sulphuric acid (0.375 vol) at 2O0C. The solution was heated to 50°C and stirred for 15h at this temperature then the solution cooled to 20°C.The volume of the solution was reduced to 25% of the initial volume by vacuum distillation. After cooling to 2O0C, TBME (5.5 vol) was added, followed by 8% aqueous NaHCO3 solution (9.4 vol) over 15 min to a pH of 7-8. After stirring for 10 min, the layers were separated and the aqueous layer was extracted with further TBME (5.5 vol). After stirring for 10 min, the layers were separated and the combined organic layers were stirred and washed with water (4.6 vol). After stirring for 10 min, the layers were separated and the organic layer was concentrated and dried at 45 - 500C to give the title compound. Yield: ca. 100% th.
References:
WO2006/134382,2006,A1 Location in patent:Page/Page column 27
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861905-21-7
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350-28-7
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861905-21-7
20 suppliers
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861905-94-4
78 suppliers
$145.00/500mg
861905-21-7
20 suppliers
$308.00/1g