1-(Aminomethyl)-3-methylenecyclobutane 97% synthesis

Yield:16333-93-0 67.1%

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran; for 2 h;Reflux;

Steps:

5.1 3-methylenecyclobutylmethylamine (Compound 4-2)

AlLiH₄ (2.45g, 64.5mmol) was dissolved in 50mL of anhydrous tetrahydrofuran, added a solution of 3-methylenecyclobutylcarbonitrile (compound 4-1) (5g, 53.7mmol) dissolved in 20mL of tetrahydrofuran, heated to reflux and stirred for 2 hours. After cooling, water (5mL, 0.7mmol) was slowly added dropwise under cooling in an ice-water bath, after the completion of addition, stirring was continued for 2 hours, and filtrated through Celite to remove insolubles. The resulting filtrate was rotary evaporated to remove solvents to give Compound 4-2 (3.5g, 67.1 % yield) .

References:

EP2738156,2014,A1 Location in patent:Paragraph 0104-0105