참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,3-Dichloroanisole | HCID 16126 | — |
| 반응물 | 4-Fluorobenzoyl chloride | HCID 67879 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,3-Dichloro-4-methoxy-4'-fluorobenzophenone | HCID 20150631 | 53.5% |
반응 단계
A mixture of 2,3-dichloroanisole (35.4 g.; 0.20 mole), 4-fluorobenzoyl chloride (34.8 g.; 0.22 mole) and methylene chloride (300 ml.) at 5° C. was stirred vigorously and treated with finely powdered aluminum chloride (28.0 g.; 0.21 mole). The reaction mixture was slowly heated and refluxed for two hours. The reaction mixture was cooled to room temperature and decomposed with ice and hydrochloric acid (50 ml.). The aqueous solution was extracted twice with methylene chloride. The combined methylene chloride solution was washed with aqueous sodium bicarbonate solution and finally with water. The organic layer was dried (MgSO4) and filtered. The solvent was removed in vacuo, and the residue on triturating with pet. ether gave the product 32 g. (50%); m.p. 138°-140°. This product was used for Step B without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04058559 |
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| 출처 데이터셋 | uspto-grants-1977_11 |
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| ORD ID | ord-e544f0f0bcf4412dbc23835a0109dfb9 |
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| 출처 메모 | uspto-grants-1977_11 |
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