참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 3-(1-bromoethyl)-7-fluoroquinoxalin-2(1H)-one | HCID 86698519 | — |
| 생성물 | 2-(1-Bromoethyl)-3-chloro-6-fluoroquinoxaline | HCID 86698520 | 92.8% |
반응 단계
A heterogeneous mixture of 3-(1-bromoethyl)-7-fluoroquinoxalin-2(1H)-one (58.86 g, 217.1 mmol) and phosphorous oxychloride (198.8 ml, 2171 mmol) in a 1 L round bottom flask was stirred at 100° C. for 2 h. The mixture was hetereogeneous in the beginning of the reaction and then homogenesous black solution over 1 h. After 2 h, the mixture was cooled to rt and concentrated under reduced pressure. To the black residue was carefully added ice (˜400 ml) in portions and then water (200 ml) with stirring. The mixture was neutralized with NH4OH (200 ml) and ice (˜200 ml) with stirring. The resulting precipitate was collected by filtration, rinsed with water (1 L), and dried under high vacuum overnight to give 2-(1-bromoethyl)-3-chloro-6-fluoroquinoxaline (58.31 g, 92.8% yield) including 3-chloro-2-(1-chloroethyl)-6-fluoroquinoxaline as a brown solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08835432B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-7424f2ef061f47c09f709f93acabcff4 |
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| 출처 메모 | uspto-grants-2014_09 |
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