반응 #43768

반응 방정식

product

N-(phenylmethyl)-3-piperidinamine

diphosgene

→

expected product

수율 30.0%

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

수율 30.0%

용매

toluene

반응 조건

후처리

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

실험 절차

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%.

출처