참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethylene Glycol | HCID 174 | — |
| 반응물 | Morpholine | HCID 8083 | — |
| 반응물 | Benzene, 1,3-diiodo- | HCID 12270 | — |
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | 4-(3-Iodophenyl)morpholine | HCID 54536434 | 41% |
반응 단계
To a solution of 1,3-diiodobenzene (5.05 g, 15.3 mmol) in isopropanol (16 mL) under nitrogen was added morpholine (1.33 g, 1.33 mL, 15.3 mmol), potassium phosphate (6.50 g, 30.6 mmol), ethylene glycol (1.90 g, 1.70 mL, 30.6 mmol) and copper (I) iodide (146 mg, 0.765 mmol). The mixture was heated at 80° C. for 15 h, and then cooled to room temperature. The solids were removed by filtration and the solution was concentrated. The residue was purified by silica gel column chromatograghy eluted with EtOAc:hexanes (5 to 25% EtOAc) to give 4-(3-iodo-phenyl)-morpholine (1.81 g, 41%) as a colorless oil. MS (ES+): m/z=290.0; 1H NMR (CDCl3, 500 MHz): δ 3.15 (t, 4H), 3.85 (t, 4H), 6.87 (dd, 1H), 6.96-7.00 (m, 1H), 7.20 (d, 1H), 7.22-7.25 (m, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07902239B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_03 |
|---|
| ORD ID | ord-4fcfbfd189614470b9d6d45029dd6011 |
|---|
| 출처 메모 | uspto-grants-2011_03 |
|---|
