反応 #77742

反応方程式

sodium bicarbonate

formic acid

acetic anhydride

ethyl 7-amino-2-chromancarboxylate

triethylamine

→

title compound

収率 100.0%

Ethyl 7-(Formylamino)chroman-2-carboxylate

収率 100.0%

溶媒

THF

反応条件

後処理

1. 1
   その他is prepared
2. 2
   その他the previously prepared
3. 3
   抽出extracted with ethyl ether
4. 4
   洗浄The combined extracts are washed with brine
5. 5
   乾燥dried over MgSO4
6. 6
   濃縮concentrated in vacuo

実験手順

Mixed anhydride is prepared by stirring 1.25 equivalents of formic acid and 1 equivalent of acetic anhydride at 60° C. for 2 h. A solution of ethyl 7-amino-2-chromancarboxylate (1.25 g; 5.6 mmol) in THF is treated with triethylamine (0.78 mL; 5.6 mmol) and the previously prepared mixed anhydride (1.6 mL), stirred at ambient temperature for 1 h, poured into a saturated aqueous solution of sodium bicarbonate and extracted with ethyl ether. The combined extracts are washed with brine, dried over MgSO4 and concentrated in vacuo to afford the title compound as a straw colored oil (1.4 g; 100%), identified by NMR spectral analysis.

出典