methyl 3,5-dihydroxy-4-iodobenzoate synthesis
- Product Name:methyl 3,5-dihydroxy-4-iodobenzoate
- CAS Number:338454-02-7
- Molecular formula:C8H7IO4
- Molecular Weight:294.04
67-56-1
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338454-02-7
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Yield: 90%
Reaction Conditions:
with sulfuric acid at 60; for 3.75 h;
Steps:
1.b Stage b) 3,5-Dihydroxy-4-iodo-benzoic acid methyl ester
3,5-Dihydroxy-4-iodo-benzoic acid (810 g; 2.89 mol) is dissolved in methanol (3,800 ml), while stirring and gassing with argon, sulphuric acid (57.5 ml) is cautiously added and the mixture is heated to 60° C. After 3 hours at this temperature, sulphuric acid (12 ml) is added again and stirring is continued for 45 minutes. After removal of the heating bath water (5,000 ml) is cautiously added and the mixture is cooled to 0° C. The crystals which have precipitated out are then filtered off with suction, washed with ice-water (2*500 ml) and dried under a high vacuum. Yield: 772 g (90%) as white crystals. M.p. 222-223° C. MS: 294 (M); 263 (M-OCH3)
References:
Basilea Pharmaceutica AG US6821980, 2004, B1 Location in patent:Page column 21
2150-44-9
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338454-02-7
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99-10-5
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338454-02-7
54 suppliers
$53.00/100mg