6-(tert-butyl)-2-chloronicotinonitrile synthesis
- Product Name:6-(tert-butyl)-2-chloronicotinonitrile
- CAS Number:4138-20-9
- Molecular formula:C10H11ClN2
- Molecular Weight:194.66
Yield:4138-20-9 83%
Reaction Conditions:
with ammonium hydrogen peroxysulfate;sulfuric acid;silver nitrate in water at 20;
Steps:
1.1 Step 1: 6-tert-butyl-2-chloro-pyridine-3-carbonitrile
Suspend 2,2-Dimethylpropionic acid (50.mL, 870mmol), 2-chloropyridine-3-carbonitrile (30g, 220mmol) and AgNO3 (9.2g, 54mmol) in 10% H2SO4 aqueous solution (300mL) in. A solution of ammonium hydrogen peroxysulfate (91 g, 430 mmol) and water (480 mL) was added dropwise to the mixture via an addition funnel. The mixture was stirred at room temperature overnight.The pH of the reaction mixture was adjusted to about 8-9 with 30% NH 4 OH (about 250 mL) and the mixture was extracted with ethyl acetate (3×300 mL). The combined organic layer was washed with brine, dried over sodium sulfate, and concentrated. The residue was subjected to silica gel column chromatography (0-25% ethyl acetate/hexane),6-tert-butyl-2-chloro-pyridine-3-carbonitrile (37g, 83%) was obtained as a clear oil,It solidified after standing.
References:
TW2017/13617,2017,A Location in patent:Page/Page column 685-686
4138-19-6
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