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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 2393057생성일: 2026년 10월 25일

Phenacyl bromide → HCID 15184924, 화합물

https://huagongshe.com/reaction/2393057

반응식

참여 물질

역할이름HCID투입량
반응물Phenacyl bromideHCID 6259—
반응물Lithium CarbonateHCID 11125—
반응물ExifoneHCID 40399—
용매DimethylformamideHCID 6228—
생성물HCID 15184924HCID 1518492437.3%

반응 조건

온도50 °C

반응 단계

3.0 g of lithium carbonate then 3.5 g of ω-bromoacetophenone are added to a solution of 5.0 g of [2,3,4-trihydroxyphenyl] [3',4',5'-trihydroxyphenyl] methanone in 20 cm3 of dimethyl-formamide maintained at 50° C., under a nitrogen atmosphere. The reaction mixture is then agitated for 6 hours at 50° C. Then 400 cm3 of a molar aceto-acetic buffer solution, the pH of which is about 4.50, are added. The resultant solution is extracted with 800 cm3 of ethyl acetate. The combined organic phases are washed with 300 cm3 of distilled water, then dried over anhydrous sodium sulphate. After filtration then evaporation to dryness under reduced pressure (2.7 kPa) at 40° C. of the ethyl acetate, 9 g of a residue are obtained and purified by chromatography on a fritted disc which contains 50 g of silica gel [eluant: dichloromethane/acetone (90/10 by volume)], collecting 30 cm3 fractions. The fractions containing the mixture of monoacetylated derivatives in position -4 and -4' are concentrated to dryness under reduced pressure (2.7 kPa), at a temperature close to 40° C. After crystallization from a dichloromethane/acetone mixture (98/2 by volume), 2.6 g of [2,3,4-trihydroxyphenyl] [3',5'-dihydroxy-4'-(2-oxo-2-phenyl-ethoxy)-phenyl] methanone is obtained in the form of a yellow powder melting at around 180° C. (with decomposition).

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US05804580
출처 데이터셋uspto-grants-1998_09
ORD IDord-529667d58c3d4b4795067026639fb66d
출처 메모uspto-grants-1998_09