6-tert-butylnicotinonitrile synthesis
- Product Name:6-tert-butylnicotinonitrile
- CAS Number:56029-45-9
- Molecular formula:C10H12N2
- Molecular Weight:160.22
677-22-5
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Yield:56029-45-9 95%
Reaction Conditions:
Stage #1: 2-bromo-5-cyanopyridinewith copper(l) iodide;lithium bromide for 0.5 h;Inert atmosphere;Schlenk technique;
Stage #2: tert-butylmagnesium chloride in tetrahydrofuran at 0; for 12 h;
Steps:
3.1 Specific steps are as follows:
(1) Add 1.83g (10mmol) of 2-bromo-5-cyanopyridine to the Schlenk bottle,Copper iodide 0.38g (2mmol),Lithium bromide 0.35g (4mmol),Blow nitrogen for 30 minutes,The mixture is dissolved in 25mL of anhydrous tetrahydrofuran at 0,Keep the temperature,Add dropwise a solution of tert-butylmagnesium chloride in tetrahydrofuran (15mL, 1M, 15mmol),Stir for 12 hours,Allow to gradually return to room temperature.After the reaction,After treatment, 2-tert-butyl-5-cyanopyridine is obtained,The yield was 95%.Using deuterated chloroform (CDCl3) as a reagent, the structure of 2-tert-butyl-5-cyanopyridine was characterized by a 500 MHz nuclear magnetic resonance instrument (hydrogen spectrum, 1H NMR).
References:
CN113087660,2021,A Location in patent:Paragraph 0135-0138
