Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzonitrile → 1-Phenyl-cyclopropylamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzonitrile | HCID 7505 | — |
| 반응물 | Boron trifluoride etherate | HCID 8000 | — |
| 반응물 | HCID 178461630 | HCID 178461630 | — |
| 촉매 | HCID 178460666 | HCID 178460666 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 1-Phenyl-cyclopropylamine | HCID 194549 | 31.5% |
반응 단계
To benzonitrile (1.03 g, 10 mmol) in ether (50 ml) at −70° C. was added Ti(OiPr)4 (3.22 ml, 11 mmol) and EtMgBr (3M in ether, 7.34 mL, 22 mmol) dropwise, the resulting yellow suspension was warmed up to room temperature over 1 h. After stirring for additional 30 min, the dark brown solution was added BF3.Et2O (2.47 mL, 20 mL) at room temperature. The mixture was further stirred for 1 h, and was quenched by 1N HCl (30 mL) and 5N NaOH (30 mL), the suspension was extracted with ether, ether layer was combined, concentrated to give crude residue, which was purified by column (Hexanes/EtOAc, 2:1 to 1:9) to give 1-phenylcyclopropanamine (420 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08853230B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-a95c49d72ce0490fafa98d752a9964c4 |
| 출처 메모 | uspto-grants-2014_10 |