反応 #62376

反応方程式

sulfamic acid

5-formylfuran-2-carboxylic acid benzyl ester

sodium chlorite

potassium dihydrogen phosphate

sodium thiosulfate

→

title compound

収率 99.2%

Furan-2,5-dicarboxylic acid monobenzyl ester

収率 99.2%

溶媒

water

acetonitrile

water

反応条件

後処理

1. 1
   workup.ADDITIONadded with a solution
2. 2
   workup.ADDITIONwas added dropwise
3. 3
   温度After cooling at this temperature for 30 minutes
4. 4
   その他the reaction
5. 5
   抽出extracted with a mixture of tetrahydrofuran and ethyl acetate
6. 6
   洗浄The organic phase was washed with water and saturated brine
7. 7
   乾燥dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONThe solvent was distilled off

実験手順

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.

出典