(Hive Bee)
04-15-03 18:21
No 426980
(Rated as: excellent)
N-Benzoyl-Morpholine (Schotten-Baumann-Style)
To a solution of 6g NaOH and 10ml of Morpholine in 46ml of Water were added 13,5ml of Benzoylchloride during a time of 1 H (magnet stirring!). The mixture was suspended in a cold waterbath to keep the temperature low.
After the addition of Benzoylchloride was finished + additional 30mins of stirring the mixture was extracted with Toluene. The toluene layer was washed twice with water, dried over Na2SO4, and distillied under vakuum.
When all the toluene had distilled over there was 10ml of oil left in the distilling flask - it wouldnt boil @ aspirator vacuum/160°C oil bath.
After cooling the flask down the contents crystallized quickly into white needles with only a very slight smell.
Yield: 10,6g (48,4% of Theory)
Any suggestions how to increase the yields? - In literature (orgsyn.org) they get ~90% for N-Benzoylpiperidine
