Ethyl Acetoacetate → 3-(2'-Oxo-3'-ethoxycarbonylbutyl)-benzophenone

Dry sodium ethylate prepared from 2.51 g of sodium was added to 125 ml of anhydrous benzene and 13.5 ml of ethyl acetylacetate at 20°C and after heating at 100°C for 15 minutes, 27.5 g of 3-bromomethyl-benzophenone were added all at once. The reaction mixture was refluxed for 3 hours and after cooling to 20°C, the benzene solution was washed twice with 25 ml of 2N hydrochloric acid and then with water until the wash water was neutral. The solution was dried over sodium sulfate and evaporated to dryness under reduced pressure to obtain 33.8 g of raw product which was chromatographed over silica gel and was eluted with a 50-50 mixture of ether-petroleum ether (B.P. of 40°-60°C) to obtain 15.3 g of 3-(2'-oxo-3'-ethoxycarbonyl-butyl)-benzophenone in the form of a marron resin which was used as is for the next step.

1. temperatureThe reaction mixture was refluxed for 3 hours
2. temperatureafter cooling to 20°C
3. washthe benzene solution was washed twice with 25 ml of 2N hydrochloric acid
4. dry with materialThe solution was dried over sodium sulfate
5. customevaporated to dryness under reduced pressure
6. customto obtain 33.8 g of raw product which
7. customwas chromatographed over silica gel
8. washwas eluted with a 50-50 mixture of ether-petroleum ether (B.P. of 40°-60°C)

ORD 기록

ord-30f4bcb783f145a99570c35c985b9f95

출처 데이터셋

uspto-grants-1976_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US03931302