참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Propionyl chloride | HCID 62324 | — |
| 반응물 | 4-Bromo-2-fluoro-1,1'-biphenyl | HCID 521063 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Carbon Disulfide | HCID 6348 | — |
| 생성물 | 1-(4'-Bromo-2'-fluorobiphenyl-4-yl)propan-1-one | HCID 822002 | 33.9% |
반응 단계
40 g of aluminum chloride and 280 ml of carbon disulfide were taken into a flask, cooled with an ice-salt bath to 0° C. or lower and stirred. A solution of 70 g of 4-bromo-2-fluorobiphenyl as dissolved in 180 ml of carbon disulfide was dropwise added thereto. A solution of 26 g of propionic acid chloride as dissolved in 100 ml of carbon disulfide was dropwise added thereto at 0° C. or lower. After addition, the whole was stirred for 2 hours at 0° C. or lower and then at room temperature overnight. After reaction, the reaction solution was poured into 30 ml of concentrated hydrochloric acid and 300 g of ice and extracted with chloroform. The organic layer was washed three times with water, two times with an aqueous 2% sodium hydroxide solution and then three times with water, and chloroform and carbon disulfide were removed by distillation. The residue was recrystallized from a mixed solvent comprising acetone and methanol to obtain 29 g of 2-fluoro-4-bromo-4'-propionylbiphenyl.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05437815 |
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| 출처 데이터셋 | uspto-grants-1995_08 |
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| ORD ID | ord-46859a31ab31461b95d8d0e940c1bb9c |
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| 출처 메모 | uspto-grants-1995_08 |
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