참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Ethyl 3-iodobenzoate | HCID 143542 | — |
| 반응물 | L-Proline | HCID 145742 | — |
| 반응물 | 3-Aminoazetidine, 3-BOC protected | HCID 1519405 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Ethyl 3-{3-[(tert-butoxycarbonyl)amino]azetidin-1-yl}benzoate | HCID 68405850 | 57.2% |
반응 단계
A suspension of 3-tert-butoxycarbonylaminoazetidine (300 mg, 1.74 mmol), ethyl 3-iodobenzoate (721 mg, 2.61 mmol) and copper (I) iodide (66 mg, 0.35 mmol), proline (80 mg, 0.70 mmol) and potassium carbonate (721 mg, 5.22 mmol) in DMSO was stirred at 120° C. for two hours. The reaction solution was diluted with ethyl acetate and then filtered. The filtrate was washed with brine and then dried over anhydrous magnesium sulfate. Following filtration, the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=4/1) to obtain 319 mg of the title compound as a milk white solid (57%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08536197B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-5a04a1605eb34951a9345797ad1dceed |
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| 출처 메모 | uspto-grants-2013_09 |
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