Reaktion #638969

Reaktionsgleichung

4-nitrophenyl 2,3-dihydro-4H-1,4-benzoxazine-4-carboxylate

3-(pyrrolidin-3-yl)pyridine

water

→

4-[(3-(pyridin-3-yl)pyrrolidin-1-yl)carbonyl]-3,4-dihydro-2H-1,4-benzoxazine

Ausbeute 92.2%

Lösungsmittel

Dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe tube is sealed
2. 2
   TrocknenThe organic phase is dried over magnesium sulfate
3. 3
   Sonstigethe solvent is evaporated under reduced pressure
4. 4
   SonstigeThe residue is chromatographed on silica gel with a dichloromethane/methanol gradient from 1/0 to 95/5

Vorschrift

0.2 g of 4-nitrophenyl 2,3-dihydro-4H-1,4-benzoxazine-4-carboxylate, 0.1 g of 3-(pyrrolidin-3-yl)pyridine and 1.5 ml of water are introduced into a 10 ml glass tube. The tube is sealed and then heated at 100° C. under microwave irradiation for 35 minutes. Dichloromethane is added. The organic phase is dried over magnesium sulfate and the solvent is evaporated under reduced pressure. The residue is chromatographed on silica gel with a dichloromethane/methanol gradient from 1/0 to 95/5. 0.19 g of 4-[(3-(pyridin-3-yl)pyrrolidin-1-yl)carbonyl]-3,4-dihydro-2H-1,4-benzoxazine is obtained.

Quelle