참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | Sodium Sulfite | HCID 24437 | — |
| 반응물 | 1-(4'-Methoxy(1,1'-biphenyl)-4-yl)ethanone | HCID 301557 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 4'-Methoxy(1,1'-biphenyl)-4-carboxylic acid | HCID 2759552 | 93.1% |
반응 단계
A solution of 64.7 g (1.61 mol) of soda in 560 ml water is prepared at 0° C. 69.9 g (0.44 mol) of bromine then 260 ml of 1,4-dioxane are added successively. A yellow solution is obtained which is cooled down to 0° C. and which is added over 10 minutes, without exceeding 10° C., to a suspension of 28 g (0.12 mol) of 4'-acetyl-4-methoxybiphenyl in a mixture of 750 ml of 1,4-dioxane and 510 ml water. The reaction medium is agitated for 1 hour at approximately 20° C., a solution of 15.5 g of sodium sulphite in 160 ml water is added and taken to reflux for 10 minutes. 76 ml of concentrated hydrochloric acid is added and the reaction medium is left under agitation whilst being cooled down, for 1 hour. After drying, washing with water and drying at 50° C., 25.5 g of 4'-methoxy-4-biphenyl carboxylic acid is obtained in the form of a white powder (yield: 93%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06160157 |
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| 출처 데이터셋 | uspto-grants-2000_12 |
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| ORD ID | ord-61b8de6292bf42d3a801a6f444ab5ebe |
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| 출처 메모 | uspto-grants-2000_12 |
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