참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium thiocyanate | HCID 516872 | — |
| 반응물 | 4-(2-Bromoethyl)-1,1'-biphenyl | HCID 6424581 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-(4-Bipenylyl)ethylthiocyanate | HCID 18333135 | 74.6% |
반응 단계
Bromine (1.5 ml) was added dropwise to an acetonitrile (60 ml) solution of triphenylphosphine (5 g). After stirring for 5 minutes, an acetonitrile solution (30 ml) of 2-(4-biphenylyl)ethanol (5 g) was added to the reaction mixture. The reaction mixture was stirred at room temperature for one hour and concentrated. Diethyl ether was added to the residue. The supernatant was collected, then dried and concentrated. The residue was purified by silica gel column chromatography (eluent: IPE) to obtain 2-(4-bipenylyl)ethylbromide(6 g). 2-(4-Bipenylyl)ethyl bromide (6 g) was dissolved in methanol (100 ml), which was stirred at 70° C. for 48 hours together with potassium thiocyanate (4.0 g). The reaction mixture was concentrated, and the residue was extracted with ethyl acetate. The organic layer was washed with water, then dried and concentrated. The residue was recrystallized from ethyl acetate-hexane to obtain the entitled compound (4.1 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06329389B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_12 |
|---|
| ORD ID | ord-51729724afe44607b0ba2feef59384a5 |
|---|
| 출처 메모 | uspto-grants-2001_12 |
|---|