G-IODOBUTYRONITRILE synthesis

Yield:6727-73-7 95%

Reaction Conditions:

with sodium iodide in acetonitrile at 60; for 1.16667 h;

Steps:

60 Preparation of 4-iodobutanenitrile

Preparation of 4-iodobutanenitrile
After 4-bromobutanenitrile (1.48 g, 10 mmol) was dissolved in acetonitrile (30 mL), sodium iodide (6 g, 40 mmol) was added thereto, and the mixture was stirred for 70 minutes at 60° C.
After the temperature was lowered to room temperature, water (30 mL) was added to the reaction material, and the result was extracted with ethyl acetate (30 mL*2).
Excess iodine was removed by washing the organic layer with a 1% aqueous sodium thiosulfate solution, and the organic layer was washed with salted water, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure to give a target compound (1.86 g, 95%).
¹H-NMR (300 MHz, CDCl₃) δ 2.13 (m, 2H), 2.53 (t, J=13.8 Hz, 2H), 3.30 (t, J=13 Hz, 2H)

References:

US2014/249162,2014,A1 Location in patent:Paragraph 0431; 0432; 0433