Reaktion #7378

Reaktionsgleichung

1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride

HOBT

triethylamine

3-amino-1-N-Boc-piperidine

DMF

DMF

→

title compound

tert-Butyl 3-(benzoylamino)piperidine-1-carboxylate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITcontinued for 18 h
3. 3
   EinengenThe solution was concentrated under reduced pressure
4. 4
   Sonstigeto give an oil which
5. 5
   Sonstigewas partitioned between ethyl acetate and water
6. 6
   WaschenThe separated organic extracts were washed with water, hydrochloric acid (2N), saturated sodium bicarbonate solution and brine
7. 7
   Trocknendried (over magnesium sulphate)
8. 8
   Einengenconcentrated under reduced pressure

Vorschrift

A solution of benzoic add (0.123 g) in DMF (5 ml) was treated with 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (0.231 g), HOBT (0.163 g) and triethylamine (0.56 ml) and stirred at room temperature for 1 h. A solution of 3-amino-1-N-Boc-piperidine (0.3 g) in DMF (1 ml) was then added and stirring continued for 18 h. The solution was concentrated under reduced pressure to give an oil which was partitioned between ethyl acetate and water. The separated organic extracts were washed with water, hydrochloric acid (2N), saturated sodium bicarbonate solution and brine, dried (over magnesium sulphate) and concentrated under reduced pressure to give the title compound (0.120 g) as a yellow solid.

Quelle