참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 5-Bromosalicylic acid | HCID 6972 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Phenyl dihydrogen orthoborate | HCID 78412 | — |
| 반응물 | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-Hydroxy[1,1'-biphenyl]-3-carboxylic acid | HCID 67584 | 89.2% |
반응 단계
In 400 ml of water, 21.7 g of 5-bromosalicylic acid, 13.41 g of phenylboric acid and 15.28 g of potassium carbonate were dissolved. The solution was stirred at room temperature for 40 minutes. After the completion of the reaction was confirmed with TLC, the reaction liquid was poured into a mixed medium of diluted hydrochloric acidethyl acetate. The mixture was extracted, and the organic phase was collected and washed with saturated sodium chloride aqueous solution. After dried with magnesium sulfate, the liquid was concentrated to form a crude product. The product was recrystallized from acetonitrile to obtain 18.58 g of 5-phenylsalicylic acid in the form of colorless crystallites. The yield was 87%. The product was confirmed with NMR and mass spectroscopy.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06726966B2 |
|---|
| 출처 데이터셋 | uspto-grants-2004_04 |
|---|
| ORD ID | ord-e14dc147047b414ba7fc96fbc80376d9 |
|---|
| 출처 메모 | uspto-grants-2004_04 |
|---|