참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Phthalic Anhydride | HCID 6811 | — |
| 반응물 | Fluorobenzene | HCID 10008 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 생성물 | 2-(4-Fluorobenzoyl)benzoic acid | HCID 82099 | 80.7% |
반응 단계
To a stirred mixture of 25 parts of 1,3-isobenzofurandione and 108.5 parts of fluorobenzene were added portionwise 50 parts of aluminium chloride. Upon completion, the whole was heated slowly to reflux and stirring was continued for 1.50 hours at reflux temperature. The reaction mixture was cooled and poured onto a mixture of crushed ice and 60 parts of concentrated hydrochloric acid. The product was extracted twice with dichloromethane. The combined extracts were washed with a sodium hydroxide solution 10%. The aqueous phase was separated, washed with 2,2'-oxybispropane and acidified with concentrated hydrochloric acid while cooling. The whole was stirred for one hour at room temperature. The precipitated product was filtered off and dissolved in benzene. The solution was distilled azeotropically to dry. The solid residue was stirred in hexane. The product was filtered off and dried in vacuo at about 50° C., yielding 33.5 parts (80.7%) of 2-(4-fluorobenzoyl)benzoic acid; mp. 129.2° C. (intermediate 7).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04766125 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-a1cb8412e9314137a5c53588cbedab76 |
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| 출처 메모 | uspto-grants-1988_08 |
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