関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Dimethylamino)-2-propenal | HCID 79125 | — |
| 反応物 | trans-4-(Dimethylamino)-3-buten-2-one | HCID 5369152 | — |
| 反応物 | Borate(1-), tetrafluoro-, hydrogen, compd. with pyridine (1:1:1) | HCID 11019233 | — |
| 溶媒 | AcOH AcOAc | HCID 21895370 | — |
| 生成物 | HCID 178467801 | HCID 178467801 | 96% |
反応手順
Pyridinium tetrafluoroborate (2.21 g, 13.3 mmol) was added to a solution of (3E)-4-(dimethylamino)-3-buten-2-one (1.54 ml, 13.3 mmol) in 13.5 ml acetic anhydride/acetic acid (2:1). The resulting suspension was cooled to 0° C. and 3-dimethylaminoacroleine (1.33 ml, 13.3 mmol) was added over a period of 1 h under vigorous stirring and cooling with an ice bath receiving a red-brown precipitate. The cool reaction mixture was filtered and the remaining solid was washed with diethylether several times and dried under reduced pressure. The pentamethinium salt was obtained as orange crude product (2.69 g, 96%) and was used without any further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08754111B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-cd552ca6e27549e988c610e8cce96ebb |
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| 出典メモ | uspto-grants-2014_06 |
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