참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Bromo-2,6-dichloroaniline | HCID 69680 | — |
| 반응물 | 4-Azido-5-fluoropyridine-3-carbaldehyde | HCID 86697053 | — |
| 촉매 | Titanium Tetrachloride | HCID 24193 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178514518 | HCID 178514518 | — |
반응 단계
A solution of 4-azido-5-fluoropyridine-3-carbaldehyde (10.0 g, 60.0 mmol) and 4-bromo-2,6-dichlorophenylamine (14.4 g, 60.0 mmol) in DCM (200 mL) was cooled to 0° C., under an atmosphere of nitrogen. Triethylamine (25 mL, 180 mmol) was added, followed by dropwise addition of titanium (IV) chloride solution (1 N in DCM, 36 mL, 36 mmol). The reaction mixture was stirred at 0° C. then allowed to reach room temperature overnight. The resultant mixture was concentrated under reduced pressure and the residue was suspended in toluene and filtered through a pad of Celite®. The filtrate was concentrated under reduced pressure to afford the title compound (quantitative yield). This was used in the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09309240B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-c59e30ddaa304666927155eca0c92fb9 |
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| 출처 메모 | uspto-grants-2016_04 |
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