참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Dodecyne | HCID 69821 | — |
| 반응물 | 5-Bromo-2-hydroxybenzene-1,3-dicarbaldehyde | HCID 5260206 | — |
| 촉매 | HCID 178419050 | HCID 178419050 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 5-(Dodec-1-YN-1-YL)-2-hydroxybenzene-1,3-dicarbaldehyde | HCID 59710865 | 46% |
반응 단계
2,6-Diformyl-4-bromophenol (2.50 g, 10.9 mmol), 1-dodecyne (2.00 g, 12.0 mmol), Cul (65 mg, 0.33 mmol), and bis(triphenylphosphine)palladium)II)dichloride were suspended in degassed acetonitrile (MeCN) (5 mL) and degassed benzene (1 mL). The yellow suspension was sparged with argon for 30 min and degassed Et3N (1 mL) was added. The resulting brown suspension was sealed in a pressure vial, warmed to 80° C. and held there for 12 h. The mixture was then partitioned between EtOAc and KHSO4 solution. The organic layer was separated, washed with brine, dried MgSO4) and concentrated under reduced pressure. The dark yellow oil was purified by column chromatography on silica gel (25% Et2O in hexanes) to give 1.56 g (46%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07563890B2 |
|---|
| 출처 데이터셋 | uspto-grants-2009_07 |
|---|
| ORD ID | ord-2fe543425c5d41608322a71ab1ccb910 |
|---|
| 출처 메모 | uspto-grants-2009_07 |
|---|