반응 #50026

반응 방정식

NaHCO3

L-pyroglutamic acid

methanol

H2SO4

→

(S)-Pyroglutamic Acid Methyl Ester

용매

THF

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도The reaction mixture was cooled to room temperature
3. 3
   workup.STIRRINGthe mixture was stirred for an additional 16 hr
4. 4
   건조The mixture was dried by addition of 314 g of Na2SO4
5. 5
   workup.STIRRINGwith stirring for 1 hr
6. 6
   여과the mixture was filtered
7. 7
   기타the solvent was evaporated under vacuum
8. 8
   기타to yield a pale yellow oil
9. 9
   여과a small amount of unreacted acid was filtered off
10. 10
    기타The THF was removed under vacuum
11. 11
    건조the residual oil was dried by azeotropic distillation with toluene

실험 절차

A 500 g sample of L-pyroglutamic acid was added to 2.8 L of anhydrous methanol, 28 mL of H2SO4 was added, and the mixture was stirred for 4 hr at 60° C. The reaction mixture was cooled to room temperature, 262 g of NaHCO3 was added, and the mixture was stirred for an additional 16 hr. The mixture was dried by addition of 314 g of Na2SO4 with stirring for 1 hr, then the mixture was filtered and the solvent was evaporated under vacuum to yield a pale yellow oil. The oil was dissolved in THF, and a small amount of unreacted acid was filtered off. The THF was removed under vacuum, and the residual oil was dried by azeotropic distillation with toluene.

출처