Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tetrahydrofuran → 4-(8-Cycloproply-2,2,4,4-tetramethyl-chroman-6-yl-ethynyl)-benzoic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 8-Cyclopropyl-6-ethynyl-2,2,4,4-tetramethylchroman | HCID 22569006 | — |
| 반응물 | Ethyl-4-iodo-benzoate benzoate | HCID 69887287 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-(8-Cycloproply-2,2,4,4-tetramethyl-chroman-6-yl-ethynyl)-benzoic acid ethyl ester | HCID 69548071 | — |
반응 단계
Following general procedure F and using 8-cyclopropyl-6-ethynyl-2,2,4,4-tetramethylchroman (Intermediate 34, 0.1 g, 0.38 mmol), ethyl-4-iodo-benzoate benzoate (Reagent A, 0.1 g, 0.34 mmol), triethyl amine (5 mL), tetrahydrofuran(10 mL), copper(I)iodide(0.025 g, 0.13 mmol) and dichlorobis(triphenylphosphine)palladium(II) (0.075 g, 0.11 mmol) followed by flash column chromatography over silica gel (230-400 mesh) using 5-10% ethyl acetate in hexane as the eluent, the title compound was obtained (0.135 g, 89%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06713647B2 |
| 출처 데이터셋 | uspto-grants-2004_03 |
| ORD ID | ord-f6ae20a07c4d46bcac2d646c87f0d300 |
| 출처 메모 | uspto-grants-2004_03 |