関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 3-Chloro-2-fluorobenzaldehyde | HCID 736335 | — |
| 反応物 | 6-Chloro-5-fluoroindolin-2-one | HCID 9794083 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Z-6-chloro-3-(3-chloro-2-fluoro-benzylidene)-5-fluoro-1,3-dihydro-indol-2-one | HCID 86653933 | 87% |
反応手順
To the mixture of 6-chloro-5-fluoroindolin-2-one (Natrochem) (2.88 g, 15.5 mmol) and 3-chloro-2-fluorobenzaldehyde (3.69 g, 23.3 mmol) (Aldrich) in methanol (140 mL) was added piperidine (3.96 g, 46.6 mmol) (Aldrich) dropwise. The mixture was then heated at 50° C. for 3 h. After cooled to 4° C., the mixture was filtered and resulting precipitate was collected, dried to give E/Z-6-chloro-3-(3-chloro-2-fluoro-benzylidene)-5-fluoro-1,3-dihydro-indol-2-one as a yellow solid (Yield 4.4 g, 87%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088815B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-d6579ea61160444eb895eee759c569ed |
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| 出典メモ | uspto-grants-2012_01 |
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