Org Prep Daily

October 9, 2006


Filed under: procedures — milkshake @ 2:57 am


1,5,7-Triazabicyclo[4,4,0]dec-5-ene 4.939g (35.48 mmol, Fluka) mixture with water 2mL and lithium hydroxide monohydrate 918mg (Aldrich) was heated in a closed pressure tube to 145C for 1 hour. The reaction mixture was purified on a short (3 inch-long) column of silica in mixture chloroform-methanol-conc. aq. ammonia 80:40:4 and the purified product was dried on highvac overnight. Y=5.265g (94%) of a white extremely hygroscopic solid.

Using the same reaction conditions and purification procedure, DBU 5.0mL (33.4mmol) and LiOH.H2O 420mg and water 2mL provided 1-(3′-aminopropyl)-caprolactam 4.973g (87%) as a colorless liquid.  

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