METHYL 3-CHLORO-4-HYDROXYBENZOATE synthesis
- Product Name:METHYL 3-CHLORO-4-HYDROXYBENZOATE
- CAS Number:3964-57-6
- Molecular formula:C8H7ClO3
- Molecular Weight:186.59
67-56-1
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3964-58-7
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3964-57-6
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Yield:3964-57-6 83%
Reaction Conditions:
with sulfuric acid at 60; for 12 h;
Steps:
[00418] Preparation of 3-Chloro-4-isopropoxybenzoic acid[00419] Step 1:[00420] To a solution of 3-chloro-4-hydroxy-benzoic acid (1.0 g, 5.8 mmol) in methanol (30 mL) was added sulfuric acid (3 mL, 56.3 mmol) and the mixture was stirred at 60 °C for 12 hours. The reaction mixture was cooled to room temperature and the methanol was removed in vacuo. The residue was partitioned between a saturated solution of 2CO3 and ethyl acetate (3 x 30 mL), dried, filtered and concentrated in vacuo to yield methyl 3-chloro-4-hydroxy-benzoate (0.9 g, 83 %) as a white solid. ESI- MS m/z calc 186.5, found 187.5 (M+l)+; Retention time: 1.17 minutes (3 min run). NMR (400.0 MHz, CDC13) δ 8.05 (d, J = 2.2 Hz, 1H), 7.90 - 7.87 (dd, J= 8.8, 2.2 H, 1H), 7.06 (d, J = 8.8 Hz, 1H) and 3.90 (s, 3H).
References:
WO2012/125613,2012,A1 Location in patent:Page/Page column 145
99-76-3
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3964-57-6
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2420-16-8
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3964-57-6
175 suppliers
$5.00/250mg