4-Chloro-5-iodo-nicotinonitrile synthesis
- Product Name:4-Chloro-5-iodo-nicotinonitrile
- CAS Number:959972-34-0
- Molecular formula:C6H2ClIN2
- Molecular Weight:264.45
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Yield:959972-34-0 75%
Reaction Conditions:
Stage #1: 4-hydroxy-5-iodopyridine-3-carbonitrilewith trichlorophosphate at 100; for 2 h;
Stage #2: with sodium hydroxide in water at 0; pH=8 - 9;
Steps:
16
A mixture of 4-hydroxy-5-iodonicotinonitrile (57.5 g, 234 mmol) and POCl3 (200 mL) was heated at 100° C. for 2 hours, cooled to room temperature and evaporated to remove excess POCl3. The residue was cooled in an ice-water bath, adjusted to pH 8-9 with aqueous 10 N NaOH and extracted with EtOAc. The combined organics were washed with water and brine, dried over MgSO4, filtered and concentrated. The resulting solid residue washed with a minimum amount of MeOH and CH2Cl2 to give 46.5 g (75%) of 4-chloro-5-iodonicotinonitrile as a tan solid, mp 120-122° C.
References:
US2007/287738,2007,A1 Location in patent:Page/Page column 24
959972-33-9
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959972-34-0
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