반응 #89014

반응 방정식

NaNO2

(S)-2-aminopentanedioic acid

HCl

→

crude product

수율 63.3%

(2S)-5-oxotetrahydrofuran-2-carboxylic acid

수율 63.3%

용매

H2O

H2O

반응 조건

후처리

1. 1
   농축The solvent was concentrated in vacuo below 50° C
2. 2
   여과filtered
3. 3
   건조The filtrate was dried over Na2SO4
4. 4
   농축concentrated in vacuo

실험 절차

To a solution of (S)-2-aminopentanedioic acid (100 g, 680 mmol) in H2O (500 mL) was added HCl (140 mL, 1.6 mol) and then NaNO2 (70.4 g, 1.02 mol) in H2O (100 mL) was added slowly at −5° C.-0° C., and the reaction mixture was stirred at room temperature for 24 hours. The solvent was concentrated in vacuo below 50° C. The residue was suspended in EtOAc (500 mL) and filtered. The filtrate was dried over Na2SO4 and concentrated in vacuo to afford 56 g crude product of (2S)-5-oxotetrahydrofuran-2-carboxylic acid (compound 28a) as yellow oil, which was used in next step without further purification.

출처