Reaktion #1446536

Reaktionsgleichung

N-iodosuccinimide

N,N-dimethylformamide

2-benzyl-6-[(3R,4R)-3,4-ethylenedioxypyrrolidine-1-yl]pyridine

→

target compound

2-Benzyl-6-[(3R,4R)-3,4-ethylenedioxypyrrolidine-1-yl]-3-iodopyridine

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGby stirring overnight as it
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   WaschenThe organic phase was successively washed with an aqueous sodium sulfite solution, water and brine
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   Sonstigethe solvent was removed
6. 6
   FiltrationThe residue was subjected to filtration
7. 7
   Sonstigecrystallized from hexane/ethyl acetate

Vorschrift

4.04 g of N-iodosuccinimide was added little by little to a solution of 40 ml of N,N-dimethylformamide containing 4.84 g of 2-benzyl-6-[(3R,4R)-3,4-ethylenedioxypyrrolidine-1-yl]pyridine under stirring in an ice bath, followed by stirring overnight as it was. The reaction solution was poured into water, and extracted with ethyl acetate. The organic phase was successively washed with an aqueous sodium sulfite solution, water and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was subjected to filtration using silica gel and crystallized from hexane/ethyl acetate, to give 5.12 g of the target compound.

Quelle