반응 #62376

반응 방정식

sulfamic acid

5-formylfuran-2-carboxylic acid benzyl ester

sodium chlorite

potassium dihydrogen phosphate

sodium thiosulfate

→

title compound

수율 99.2%

Furan-2,5-dicarboxylic acid monobenzyl ester

수율 99.2%

용매

water

acetonitrile

water

반응 조건

후처리

1. 1
   workup.ADDITIONadded with a solution
2. 2
   workup.ADDITIONwas added dropwise
3. 3
   온도After cooling at this temperature for 30 minutes
4. 4
   기타the reaction
5. 5
   추출extracted with a mixture of tetrahydrofuran and ethyl acetate
6. 6
   세척The organic phase was washed with water and saturated brine
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONThe solvent was distilled off

실험 절차

490 mg of 5-formylfuran-2-carboxylic acid benzyl ester was dissolved in 10 mL of acetonitrile, and added with a solution containing 413 mg of sulfamic acid in 5 mL of water. After cooling to 0° C., a solution containing 202 mg of sodium chlorite and 232 mg of potassium dihydrogen phosphate in 5 mL of water was added dropwise. After cooling at this temperature for 30 minutes, sodium thiosulfate aqueous solution was added at 0° C. to stop the reaction, and extracted with a mixture of tetrahydrofuran and ethyl acetate. The organic phase was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off to afford 520 mg of the title compound as white crystals.

출처