4-Chloro-3-iodo-2-methyl-pyridine synthesis
- Product Name:4-Chloro-3-iodo-2-methyl-pyridine
- CAS Number:1227515-08-3
- Molecular formula:C6H5ClIN
- Molecular Weight:253.47
1226880-00-7
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1227515-08-3
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Yield:1227515-08-3 83%
Reaction Conditions:
with phosphorous pentoxide;trichlorophosphate in acetonitrile; for 3 h;Reflux;
Steps:
1.2.2 Step 2: 4-chloro-3-iodo-2-methylpyridine
To a solution of 3-iodo-2-methylpyridin-4-ol (6.25 g, 26.1 mmol) in ACN (30 mL) were added slowly POCl3 (18.16 g, 117 mmol) and P2O5 (154 mg, 1.04 mmol). The reaction mixture was stirred under reflux for 3 hours, then cooled to RT and concentrated to ca.8 mL. The residue was treated carefully with water (70 mL) with external cooling to keep the internal temperature below 45 °C. The precipitate formed was removed by filtration. The pH of the mixture was adjusted to pH = 6-7 with sodium hydroxide, the solid was filtered, washed with water and dried on high vacuum to yield title compound (5.6 g, 83 % yield) as a beige solid. LC-MS: Rt = 0.99 min; MS m/z = 254.0 [MH]+ (Method 1).
References:
WO2022/91056,2022,A1 Location in patent:Page/Page column 48-49
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1227515-08-3
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