Reaktion #351785

Reaktionsgleichung

sodium carbonate

methyl (6R)-1,6-dibenzyl-2,4-dioxo3-piperidine carboxylate

acetic acid

→

title compound

(6R)-1,6-Dibenzyl-2,4-piperidinedione

Lösungsmittel

—

ice water

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe phases are separated
2. 2
   Extraktionthe aqueous phase is extracted once more with 300 ml of ethyl acetate
3. 3
   WaschenThe combined organic phases are washed with water
4. 4
   Trocknenwith brine dried over sodium sulfate
5. 5
   Sonstigeevaporated to dryness
6. 6
   SonstigeThe resulting oil is crystallised from ether

Vorschrift

A solution of 106.1 g (0.301 mol) of methyl (6R)-1,6-dibenzyl-2,4-dioxo3-piperidine carboxylate in 298 ml of toluene and 445 ml of 10% strength (vol/vol) acetic acid is heated at 80° for 21/2 hours. The reaction mixture is cooled to room temperature, neutralised by adding 48 g of solid sodium carbonate while cooling in ice-water, the phases are separated, and the aqueous phase is extracted once more with 300 ml of ethyl acetate. The combined organic phases are washed with water, then with brine dried over sodium sulfate and evaporated to dryness. The resulting oil is crystallised from ether, resulting in the title compound.

Quelle