反応 #1870

反応方程式

2-aminobenzophenone

sodium hydrogencarbonate

→

2-(5-oxotetrahydrofuran-2-carbonyl)aminobenzophenone

溶媒

ethyl acetate

反応条件

後処理

1. 1
   洗浄The ethyl acetate layer was washed with water
2. 2
   乾燥dried over anhydrous magnesium sulfate
3. 3
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
4. 4
   その他The residue was purified by means of a silica gel column chromatography (eluent, hexane:ethyl acetate=2:1)

実験手順

A mixture of 4.9 g of 5-oxotetrahydrofuran-2-carboxylic acid and 5.5 ml of thionyl chloride was subjected to reflux for 2 hours. Thionyl chloride was then distilled off under reduced pressure to leave 5-oxotetrahydrofuran-2-carbonyl chloride. This product was mixed with 5.0 g of 2-aminobenzophenone, 200 ml of ethyl acetate and 200 ml of a saturated aqueous solution of sodium hydrogencarbonate, which was stirred for one hour at room temperature. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate, then the solvent was distilled off under reduced pressure. The residue was purified by means of a silica gel column chromatography (eluent, hexane:ethyl acetate=2:1) to give 2-(5-oxotetrahydrofuran-2-carbonyl)aminobenzophenone (6.5 g) as needles, m.p. 100° C.-102° C.

出典