Reaktion #43768

Reaktionsgleichung

product

N-(phenylmethyl)-3-piperidinamine

diphosgene

→

expected product

Ausbeute 30.0%

6-(phenylmethyl)-1,6-diazabicyclo[3,2,1]octan-7-one

Ausbeute 30.0%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITThen the temperature is left
2. 2
   Temperaturmaintained for 2 hours at 20° C
3. 3
   EinengenThe reaction medium is concentrated under reduced pressure
4. 4
   Sonstigethe residue is chromatographed on silica eluting successively with methylene chloride-acetone 95/5

Vorschrift

1.06 g of the product obtained in stage C is dissolved in 28 cm3 of toluene, then cooled down to 0° C. and 337 μl of diphosgene is added under an inert gas. Then the temperature is left to rise and maintained for 2 hours at 20° C. The reaction medium is concentrated under reduced pressure then the residue is chromatographed on silica eluting successively with methylene chloride-acetone 95/5 then 80/20 and finally methylene chloride-methanol, triethylamine 92/8/3 and 362 mg of expected product C13H16N2O (M=216.85 g) is obtained i.e. a yield of 30%.

Quelle