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HRID 546733作成日:2026年10月25日

Diisopropylethylamine → HCID 66839205、化合物

https://huagongshe.com/reaction/546733

反応式

関与物質

役割名称HCID仕込み量
反応物DiisopropylethylamineHCID 81531—
反応物Bis(2-oxo-3-oxazolidinyl)phosphinic chlorideHCID 152842—
反応物(E)-3-[3-methoxy-4-(4-methylimidazol-1-yl)phenyl]acrylic acidHCID 59528030—
反応物HCID 66839680HCID 66839680—
溶媒WaterHCID 962—
溶媒DichloromethaneHCID 6344—
生成物HCID 66839205HCID 6683920542.7%

反応手順

IPEA (2.0 mL), (E)-3-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]acrylic acid (600 mg) and BOPCl (0.71 g) were added to a solution of 5-hydroxy-3-phenylpentanoic acid hydrazide (492 mg) in methylene chloride (20 mL) at room temperature, and the reaction solution was stirred at room temperature for seven hours. Water was added to the reaction solution, followed by extraction with chloroform. The resulting extract was washed with a saturated sodium bicarbonate solution. The resulting organic layer was dried over magnesium sulfate and then concentrated under reduced pressure. Phosphorus oxychloride (10 mL) was added to the resulting residue at room temperature, and the reaction solution was heated under reflux for 1.5 hours. The reaction solution was left to cool to room temperature and then concentrated under reduced pressure. A saturated sodium bicarbonate solution was added to the residue, followed by extraction with ethyl acetate. The resulting extract was dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: heptane-ethyl acetate system) to obtain 445 mg of the title compound. The property value of the compound is as follows.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07935815B2
出典データセットuspto-grants-2011_05
ORD IDord-a396c7f2c8564eea8734624bd74ac2be
出典メモuspto-grants-2011_05