ChemicalBook CAS DataBase List Methyl 3-hydroxythiophene-2-carboxylate

Methyl 3-hydroxythiophene-2-carboxylate synthesis

6synthesis methods

Product Name:Methyl 3-hydroxythiophene-2-carboxylate
CAS Number:5118-06-9
Molecular formula:C6H6O3S
Molecular Weight:158.18

5788-17-0
149 suppliers
$21.00/5mL

2365-48-2 Synthesis

2365-48-2
348 suppliers
$15.00/25g

5118-06-9
198 suppliers
$11.00/1g

Yield:5118-06-9 88.2%

Reaction Conditions:

with sodium methylate in methanol under 7500.75 - 15001.5 Torr; for 1 h;

Steps:

1-17 Example 1
The dry clean continuous reactor was heated to 100 °C. Take methyl thioglycolate (91.4g, 0.86mol) and methanol (150g) was placed in a feed flask hit, taking a 30% sodium methoxide in methanol (232.7g, 1.29mol) was placed in flask 2 hits the material, E-3-methoxymethyl acrylate (50.0 g, 0.43 mol) and methanol (150 g) were placed in a shot bottle 3. After the temperature of the continuous coil reactor is stabilized, the material is started, and the feed rate of the shot bottle is set to 10.57 g/min. The feed rate of the shot bottle 2 was set to 0.55 g/min, and the feed rate of the shot bottle 3 was set to 0.47 g/min. The reaction zone retention time is 1 h, and the internal pressure of the continuous coil reactor is controlled at 1.0 to 2.0 MPa. The reaction system was directly passed through a hydrogen chloride/methanol solution, and quenched at a temperature of 0 to 10 °C.After completion of the quenching, the system was concentrated under reduced pressure to give methanol. The residue was purified by distillation under reduced pressure to give 60.1 g of pure white solids, purity 99.5%, yield 88.2 %

References:

Kailaiying Pharmaceutical Group (Tianjin) Co., Ltd.;Hong Hao;Lu Jiangping;Zhang Enxuan;Shen Wei;Guo Pengpeng;Song Di CN109265437, 2019, A Location in patent:Paragraph 0034-0071

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80-63-7 Synthesis