반응 #1870

반응 방정식

2-aminobenzophenone

sodium hydrogencarbonate

→

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

용매

ethyl acetate

반응 조건

후처리

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

실험 절차

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.

출처