Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tetrahydrofuran → HCID 178445732, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 반응물 | (R)-4-(6-hydroxynaphthalen-2-yl)-4-methyloxazolidin-2-one | HCID 51066623 | — |
| 반응물 | HCID 178445814 | HCID 178445814 | — |
| 생성물 | HCID 178445732 | HCID 178445732 | 88.3% |
반응 단계
A mixture of trans-4-butyl-cyclohexanol (441 mg, 2.82 mmol), ((R)-4-(6-hydroxynaphthalen-2-yl)-4-methyloxazolidin-2-one (572.5 mg, 2.353 mmol) and triphenylphosphine (741 mg, 2.82 mmol) in tetrahydrofuran (20 mL, 0.3 mol) was heated to reflux, and diisopropyl azodicarboxylate (0.556 mL, 2.82 mmol) was added dropwise. The reaction was stirred and refluxed for 3 hours. TLC and LCMS monitoring showed the reaction to be incomplete. The mixture was concentrated and taken up into dichloromethane and subjected to chromatography purification with EtOAc/hexane (10:90 to 80:20) to give product (0.793 g, 88% yield). LCMS 2.35 min (382.93, [M+1], 100%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08269043B2 |
| 출처 데이터셋 | uspto-grants-2012_09 |
| ORD ID | ord-d38c3ea3fdee43ab892e5499f1056a50 |
| 출처 메모 | uspto-grants-2012_09 |