참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Di-tert-butyl Iminodicarboxylate | HCID 279800 | — |
| 반응물 | 3-(Bromomethyl)-6-phenylpyridazine | HCID 66717445 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-[Bis(tert-butoxycarbonyl)aminomethyl]-6-phenylpyridazine | HCID 66717700 | 97% |
반응 단계
To a solution of 3-bromomethyl-6-phenylpyridazine (120 mg, 0.482 mmol) obtained in Reference Example 2-(a) in N,N-dimethylformamide (1.57 ml) were added di-tert-butyl iminodicarboxylate (127 mg, 0.585 mmol) and potassium carbonate (134 mg, 0.970 mmol), followed by stirring at 50° C. for 2 hours. After completion of the reaction, water was added to the reaction solution, followed by extraction with ethyl acetate. The separated organic layer was dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography (eluent; hexane:ethyl acetate=2:1→1:1 (UV)), and fractions containing the desired compound were concentrated under reduced pressure to afford the title compound (180 mg) as a slightly yellow solid. (Yield: 97%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08648097B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-525449ba40e64f23bc7080829e42cd68 |
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| 출처 메모 | uspto-grants-2014_02 |
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