Reacción #10514

Ecuación de reacción

tert-butyl acetate

L-pyroglutamic acid

perchloric acid

NaOH

→

tert-butyl (S)-5-oxopyrrolidine-2-carboxylate

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaIt was cooled to 0° C.
2. 2
   OtroThe phases were separated
3. 3
   Lavadothe organic phase was washed twice with 300 ml of a saturated sodium chloride solution each time
4. 4
   SecadoThe organic phase was then dried with sodium sulfate
5. 5
   OtroThe solvents were removed in vacuo
6. 6
   workup.STIRRINGthe residue was stirred with heptane
7. 7
   OtroThe solid obtained in this way
8. 8
   Filtraciónwas filtered off with suction
9. 9
   ConcentraciónThe mother liquor was concentrated in vacuo
10. 10
    Otrothe solid obtained in this way
11. 11
    Filtraciónwas also filtered off with suction

Procedimiento

129 g of L-pyroglutamic acid were suspended in 2 l of tert-butyl acetate. 30 ml of a 70% strength solution of perchloric acid in water were added thereto. The mixture was then stirred at room temperature for 12 h. It was cooled to 0° C. and the pH of the solution was adjusted to 7 by cautious addition of a 2N NaOH solution. The phases were separated and the organic phase was washed twice with 300 ml of a saturated sodium chloride solution each time. The organic phase was then dried with sodium sulfate. The solvents were removed in vacuo, and the residue was stirred with heptane. The solid obtained in this way was filtered off with suction. The mother liquor was concentrated in vacuo, and the solid obtained in this way was also filtered off with suction.

Fuente