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HRID 1737290作成日:2026年10月27日

Sodium hydride → 1,1-Bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropane

https://huagongshe.com/reaction/1737290

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium hydrideHCID 24758—
反応物Ammonium ChlorideHCID 25517—
反応物Tetraisopropyl methylenediphosphonateHCID 74266—
反応物2-Bromoethyl trityl etherHCID 10959531—
溶媒TolueneHCID 1140—
溶媒Ethyl AcetateHCID 8857—
生成物1,1-Bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropaneHCID 2184199877.4%

反応条件

温度120 °C

反応手順

Under a nitrogen atmosphere, 60% sodium hydride (200 mg), 1-bromo-2-triphenylmethoxyethane (1.84 g) and tetraisopropyl methylenebisphosphonate (1.72 g) were suspended in toluene (5 ml), and the resulting suspension was stirred at 120° C. for 7 hours. The reaction mixture was diluted with toluene, and then a saturated aqueous ammonium chloride solution was added thereto to decompose the excess sodium hydride. Then, ethyl acetate was added thereto to effect separation, and the organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by a silica gel column chromatography (chloroform:acetone) to obtain 1,1-bis(diisopropoxyphosphinoyl)-3-triphenylmethoxypropane (2.44 g, yield 77%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05962438
出典データセットuspto-grants-1999_10
ORD IDord-3d253bd6539e4ec89bb0faf99b9f6fb4
出典メモuspto-grants-1999_10