Methyl 4,6-dichloropyridazine-3-carboxylate synthesis
- Product Name:Methyl 4,6-dichloropyridazine-3-carboxylate
- CAS Number:372118-01-9
- Molecular formula:C6H4Cl2N2O2
- Molecular Weight:207.01
372118-00-8
76 suppliers
$39.00/100mg
372118-01-9
183 suppliers
$11.00/250mg
Yield:372118-01-9 72%
Reaction Conditions:
with trichlorophosphate at 95; for 5 h;
Steps:
17.3 4,6-Dichloro-pyridazine-3-carboxylic acid methyl ester
Step 3
4,6-Dichloro-pyridazine-3-carboxylic acid methyl ester
A mixture of 4,6-dihydroxy-pyridazine-3-carboxylic acid methyl ester (10.5 g, 61.7 mmol) and POCl3 (70 mL) was heated to 95° C. for 5 h.
The excess POCl3 was removed under reduced pressure, then the crude residue was added to ice-water (250 mL) and extracted with ethyl acetate (3*100 mL).
The combined extracts were dried then concentrated to give a crude residue which was purified by chromatography (silica, 100-200 mesh, 30% ethyl acetate in hexane) to give 4,6-dichloro-pyridazine-3-carboxylic acid methyl ester (9.2 g, 72%) as an off white solid. LC-MS: 207.0 [M+H]+.
References:
Hoffman-La Roche Inc.;Hermann, Johannes Cornelius;Kennedy-Smith, Joshua;Lucas, Matthew C.;Padilla, Fernando;Soth, Michael US2013/178478, 2013, A1 Location in patent:Paragraph 0301;0302
1830-54-2
401 suppliers
$9.00/10g
372118-01-9
183 suppliers
$11.00/250mg
83878-89-1
3 suppliers
inquiry
372118-01-9
183 suppliers
$11.00/250mg