Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → HCID 59401133, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 3-Quinuclidinol, (+)- | HCID 736411 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 반응물 | (R)-(4-fluoro-phenylamino)-phenyl-acetic acid | HCID 7006576 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 59401133 | HCID 59401133 | 79.2% |
반응 단계
To a solution of (R)-(4-fluoro-phenylamino)-phenyl-acetic acid (I253) (420 mg, 1.71 mmol) in dry THF (40 mL), are sequentially added (S)-quinuclidin-3-ol (218 mg, 1.71 mmol), DEAD (407 ul, 2.57 mmol) and triphenylphosphine (674 mg, 2.57 mmol). The reaction is refluxed for 30 minutes under N2 flowstream and then the solvent is evaporated. The residue is partitioned between water and EtOAc, the organic layer is separated, dried over Na2SO4, filtered and evaporated to dryness. The resulting crude is purified by flash chromatography (DCM/MeOH=95/5) to obtain the title compound as a pale yellow oil (480 mg, 79% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08835682B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-dc805f9e25c4444591a87322ff5bb48d |
| 출처 메모 | uspto-grants-2014_09 |