関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 1-Tetralone | HCID 10724 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | N-(dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate | HCID 86743575 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Diisopropyl Ether | HCID 7914 | — |
| 生成物 | HCID 53777110 | HCID 53777110 | 33.5% |
反応手順
α-Tetralone (51 g) is added dropwise in the course of 45 minutes, at a temperature in the region of 15° C., to a mixture of N-(3-dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate (100 g) in ethanol (500 cc) and a 2M ethanolic solution of sodium ethylate (210 cc). The mixture is maintained for 1 hour 45 minutes at a temperature in the region of 20° C. and is then heated for 4 hours 45 minutes to 70° C. The reaction ethanol is evaporated off to dryness and the oil obtained is pounded with ethyl ether (4×300 cc). The ethereal extracts are concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa). After recrystallization of the solid obtained in a boiling mixture (60 cc) of isopropyl ether and ethyl acetate (90:10 by volume), ethyl 2-dimethylamino-4-(1-oxo-1,2,3,4-tetrahydro-2-naphthylidene)-2-butenoate (17.5 g), m.p. 84° C., is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04886835 |
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| 出典データセット | uspto-grants-1989_12 |
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| ORD ID | ord-9c589d637e044b4ea5c51eaf5dac36c2 |
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| 出典メモ | uspto-grants-1989_12 |
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