Реакция #62376

Уравнение реакции

sulfamic acid

5-formylfuran-2-carboxylic acid benzyl ester

sodium chlorite

potassium dihydrogen phosphate

sodium thiosulfate

→

title compound

Выход 99.2%

Furan-2,5-dicarboxylic acid monobenzyl ester

Выход 99.2%

Растворители

water

acetonitrile

water

Условия реакции

Обработка

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

Методика

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.

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