Diphosgene → 6-(Phenylmethyl)-1,6-diazabicyclo[3,2,1]octan-7-one
Reaktionsgleichung
[C:1]1([CH2:7][NH:8][CH:9]2[CH2:14][CH2:13][CH2:12][NH:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[O:15]=[C:16](Cl)OC(Cl)(Cl)Cl>C1(C)C=CC=CC=1>[C:1]1([CH2:7][N:8]2[C:16](=[O:15])[N:11]3[CH2:10][CH:9]2[CH2:14][CH2:13][CH2:12]3)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
1.06 g of product obtained in Stage C is dissolved in 28 cm3 of toluene, then the reaction medium is cooled down to 0° C. and 337 μl of diphosgene is added under an inert gas. The temperature is allowed to rise and is maintained at 20° C. for 2 hours. Concentration is carried out 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%.