참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 4'-Iodobiphenyl-4-carboxylic acid | HCID 816730 | — |
| 반응물 | 4-Pentyloxyphenylboronic Acid (contains varying amounts of Anhydride) | HCID 4684888 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Poly(ethylene glycol) dimethyl ether (NHD) | HCID 445171 | — |
| 생성물 | 4''-n-Pentoxy-[1,1':4',1'']-terphenyl-carboxylic acid | HCID 23508759 | — |
반응 단계
32.4 g of 4′-iodobiphenyl-4-carboxylic acid are introduced together with 25.8 g of glycol ester of 4-n-pentoxyphenylboronic acid and 15.9 g of sodium carbonate into 300 ml of methanol/ethylene glycol 9:1 and, while stirring vigorously, 70 mg of PdCl2(PPh3)2 are added, and the mixture is stirred under reflux for 6 hours. The hot reaction mixture is cautiously poured into a mixture of 30 g of 37% strength sulfuric acid and 200 g of water, and the mixture is heated at 90-100° C. for 30 minutes. After filtration and washing with water, the crude product is dried at 80° C./100 bar and then recrystallized from dimethylacetamide. This affords after drying 28.9 g (80%) of 4″-n-pentoxy-[1,1′:4′,1″]-terphenyl-4-carboxylic acid with a purity of >99%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06762315B1 |
|---|
| 출처 데이터셋 | uspto-grants-2004_07 |
|---|
| ORD ID | ord-e00d326f7d3248f486dd4b004ac98506 |
|---|
| 출처 메모 | uspto-grants-2004_07 |
|---|
