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HRID 477302作成日:2026年10月24日

Diethyl Ether → HCID 53777110、化合物

https://huagongshe.com/ja/reaction/477302

反応式

関与物質

役割名称HCID仕込み量
反応物Diethyl EtherHCID 3283—
反応物1-TetraloneHCID 10724—
反応物Sodium ethoxideHCID 2723922—
反応物N-(dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborateHCID 86743575—
溶媒EthanolHCID 702—
生成物Diisopropyl EtherHCID 7914—
生成物HCID 53777110HCID 5377711033.5%

反応条件

温度20 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US04886835
出典データセットuspto-grants-1989_12
ORD IDord-9c589d637e044b4ea5c51eaf5dac36c2
出典メモuspto-grants-1989_12