참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 4'-Chloro-4-biphenylol | HCID 91589 | — |
| 반응물 | tert-Butyl 3-(hydroxymethyl)piperidine-1-carboxylate | HCID 2763851 | — |
| 반응물 | ethyl (NE)-N-ethoxycarbonyliminocarbamate;toluene | HCID 87147022 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 58992609 | HCID 58992609 | 67% |
반응 단계
1-(tert-Butoxycarbonyl)piperidin-3-ylmethanol (323 mg, 1.50 mmol) and 4′-chloro-4-hydroxybiphenyl (307 mg, 1.50 mmol) were suspended in tetrahydrofuran (15 mL). To this suspension, triphenylphosphine (608 mg, 2.25 mmol) was added and the mixture was stirred at room temperature for 10 min. A 40% diethylazodicarboxylate/toluene solution (1.36 mL, 3.00 mmol) was then added and the mixture was stirred at room temperature for 16 hours. Subsequently, water was added and the mixture was extracted with ethyl acetate. The extract washed with brine, followed by drying over magnesium sulfate and evaporation of the solvent. Purification of the resulting residue by silica gel column chromatography (hexane:ethyl acetate=50:1->10:1) gave 401 mg (67%) of the desired compound as a colorless powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07902367B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_03 |
|---|
| ORD ID | ord-d32fc68c954446ddb5732ec013f856ee |
|---|
| 출처 메모 | uspto-grants-2011_03 |
|---|
