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HRID 348503作成日:2026年10月27日

Dimethylformamide → 3-(5,5-Dimethyl-1,3-dioxan-2-yl)-1-(4-ethoxyphenyl)butan-1-one

https://huagongshe.com/reaction/348503

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Neopentyl glycolHCID 31344—
反応物2-Bromo-1-(4-ethoxyphenyl)ethanoneHCID 2113060—
反応物N,N-Bis(2-methylpropyl)prop-1-en-1-amineHCID 54063094—
溶媒WaterHCID 962—
生成物3-(5,5-Dimethyl-1,3-dioxan-2-yl)-1-(4-ethoxyphenyl)butan-1-oneHCID 1172269873.4%

反応手順

2-Bromo-1-(4-ethoxyphenyl)ethan-1-one (4.0 g) and N,N-bis(2-methylpropyl)-1-propenylamine (4.0 g) were added to 16 ml of dimethylformamide under an atmosphere of nitrogen and the mixture was stirred between 50° C. and 55° C. for 2 hours. To the reaction mixture were added successively 1.6 g of paratoluenesulfonic acid and 2.1 g of neopentyl glycol and the mixture was stirred between 50° C. and 60° C. for 3 hours. After addition of 8 ml of water to the reaction mixture and cooling the reaction mixture to the room temperature, crystals precipitated. These crystals were isolated by filtration to give 3.7 g (yield 72%) of the title compound as white crystals. The 1H-NMR spectrum of the product is substantially identical with that of the product of Example 1.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07176323B2
出典データセットuspto-grants-2007_02
ORD IDord-73a82ee9d658472f99a72f6156eaee4e
出典メモuspto-grants-2007_02