반응 #10514

반응 방정식

tert-butyl acetate

L-pyroglutamic acid

perchloric acid

NaOH

→

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

용매

water

반응 조건

후처리

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

실험 절차

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.

출처