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HRID 342626作成日:2026年10月27日

Potassium bisulfate → tert-butyl N-[(2S)-1-oxo-3-phenylpropan-2-yl]carbamate

https://huagongshe.com/reaction/342626

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium bisulfateHCID 516920—
反応物1,1-Dimethylethyl N-((1S)-2-(methoxymethylamino)-2-oxo-1-(phenylmethyl)ethyl)carbamateHCID 11055945—
反応物Aluminium lithium hydrideHCID 21226445—
溶媒WaterHCID 962—
溶媒Diethyl EtherHCID 3283—
生成物tert-butyl N-[(2S)-1-oxo-3-phenylpropan-2-yl]carbamateHCID 6998013—

反応条件

温度-45 °C

反応手順

A mechanically stirred suspension of lithium aluminum hydride (6.59 g, 0.165 mol) in ether (1 L) was cooled to -45° C. under nitrogen. A solution of the product from Step A (0.150 mol) in ether (150 mL) was added, maintaining the temperature below -35° C. When the addition was complete, the reaction was warmed to 5° C., then recooled to -45° C. A solution of potassium hydrogen sulfate (36.1 g, 0.265 mol) in water was slowly added, maintaining the temperature below -5° C. After quenching, the reaction was stirred at room temperature for 1 h. The mixture was filtered through Celite, the ether evaporated, and the remainder partitioned between ethyl acetate and 2% potassium hydrogen sulfate. After washing with saturated brine, drying over magnesium sulfate and solvent removal, the title compound was obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05859012
出典データセットuspto-grants-1999_01
ORD IDord-9076447184b9488f8a35983007bd93a5
出典メモuspto-grants-1999_01