Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → HCID 178445742, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 반응물 | Tert-butyl 5-(6-hydroxynaphthalen-2-yl)-2,2-dimethyl-1,3-dioxan-5-ylcarbamate | HCID 44228963 | — |
| 반응물 | HCID 178445814 | HCID 178445814 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178445742 | HCID 178445742 | — |
반응 단계
[5-(6-Hydroxynaphthalen-2-yl)-2,2-dimethyl-1,3-dioxinan-5-yl]-carbamic acid tert-butyl ester (Example 13, 498 mg, 0.00133 mol, Apex), PS-triphenylphosphine (3.00 mmol/g loading, 689 mg, 0.00207 mol, Aldrich) were slurried in Tetrahydrofuran (10 mL, Acros), then trans-4-butylcyclohexanol (0.255 g, 0.00163 mol, Synthon) and diisopropyl azodicarboxylate (0.315 mL, 0.00160 mol, Acros) was added. The reaction was stirred at room temperature. After 4 d, the mixture was diluted with ethyl acetate, filtered and concentrated and the crude product was taken up into methylene chloride and subjected to silica gel chromatography purification to give the title compound in 353 mg yield (52%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08546359B2 |
| 출처 데이터셋 | uspto-grants-2013_10 |
| ORD ID | ord-60b5840853cc4b0695cc28f71ac36825 |
| 출처 메모 | uspto-grants-2013_10 |