Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylamine → 1-(4-Trimethylsilanylethynylphenyl)propan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylamine | HCID 7912 | — |
| 반응물 | Trimethylsilylacetylene | HCID 66111 | — |
| 반응물 | p-Bromopropiophenone | HCID 66312 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(4-Trimethylsilanylethynylphenyl)propan-1-one | HCID 67363127 | — |
반응 단계
A mixture of 1.74 g 4′-bromopropiophenone, 2.0 g ethynyltrimethylsilane, 260 mg bis(triphenylphosphine)palladium(II) dichloride, 260 mg copper(I) iodide and 15 ml diisopropylamine in 40 ml tetrahydrofuran is heated at reflux for 1 h. After cooling the reaction mixture is diluted with water and extracted with ethyl acetate. The combined organic layer is washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue is purified by chromatography on silica gel, using a mixture of heptane/ethyl acetate 9:1 as eluent to obtain 1-(4-trimethylsilanylethynylphenyl)propan-1-one, m.p. 36-37° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08658644B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-3b2f550dab3f4c0b9c363fa1b256f8ef |
| 출처 메모 | uspto-grants-2014_02 |