تفاعل #50026

معادلة التفاعل

NaHCO3

L-pyroglutamic acid

methanol

H2SO4

→

(S)-Pyroglutamic Acid Methyl Ester

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   درجة الحرارةThe reaction mixture was cooled to room temperature
3. 3
   workup.STIRRINGthe mixture was stirred for an additional 16 hr
4. 4
   تجفيفThe mixture was dried by addition of 314 g of Na2SO4
5. 5
   workup.STIRRINGwith stirring for 1 hr
6. 6
   ترشيحthe mixture was filtered
7. 7
   أخرىthe solvent was evaporated under vacuum
8. 8
   أخرىto yield a pale yellow oil
9. 9
   ترشيحa small amount of unreacted acid was filtered off
10. 10
    أخرىThe THF was removed under vacuum
11. 11
    تجفيفthe residual oil was dried by azeotropic distillation with toluene

الإجراء التجريبي

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.

المصدر