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 | Borate(1-), tetrafluoro-, hydrogen, compd. with pyridine (1:1:1) | HCID 11019233 | — |
| 反応物 | AcOH AcOAc | HCID 21895370 | — |
| 生成物 | HCID 178500406 | HCID 178500406 | 65% |
反応手順
Pyridiniumtetrafluoroborate (283.7 g, 1.70 mol) was added to a solution of methyl-(2E)-3-(3-dimethylamino)prop-2-enoate in 442.5 ml acetic anhydride/acetic acid (2:1). The resulting suspension was cooled to 0° C. and 3-dimethylaminoacroleine (169.9 ml, 1.70 mol) was added slowly over the course of 3 hrs. under vigorous stirring and cooling with an ice bath, a yellow-brown precipitate formed. After further stirring for 2 hrs. at room temperature the reaction mixture was filtered. The remaining solid was washed with diethylether several times and dried under reduced pressure. Re crystallization from i-propanol/ethanol (2:1) gave 326.7 g (65%) of the pentamethinium salt as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08580949B2 |
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| 出典データセット | uspto-grants-2013_11 |
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| ORD ID | ord-a5d6e144d551412a9f4896dbda643d07 |
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| 出典メモ | uspto-grants-2013_11 |
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