Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chlorodicyclohexylphosphine → 2-(Dicyclohexylphosphino)-2'-methoxybiphenyl
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chlorodicyclohexylphosphine | HCID 2734135 | — |
| 반응물 | 3-Methyl-1,1-bis(4-methylphenyl)-2-butanone | HCID 12040744 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(Dicyclohexylphosphino)-2'-methoxybiphenyl | HCID 11794186 | 54.4% |
반응 단계
A solution of 1 (535 mg, 2.03 mmol) in THF (20 mL) was cooled to −78° C. under argon, then n-BuLi (1.6 M in hexane, 1.35 mL, 2.16 mmol) was added dropwise. After 2.5 h at −78° C., a solution of chlorodicyclohexylphosphine (570 mg, 2.45 mmol) in THF (3 mL) was added over 10 min. The reaction mixture was then allowed to warm to room temperature overnight, then quenched with saturated aqueous NaHCO3 and concentrated in vacuo. The resulting aqueous suspension was extracted with ether (2×50 mL), and the combined ethereal layers were dried (Na2SO4), filtered and concentrated in vacuo. The resulting crude solid was recrystallized from ethanol to afford 420 mg (54%) of a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06946560B2 |
| 출처 데이터셋 | uspto-grants-2005_09 |
| ORD ID | ord-2aac3abf10d6404c9f7ff39698b50a7e |
| 출처 메모 | uspto-grants-2005_09 |