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HRID 11488作成日:2026年10月25日

Sodium Sulfite → 1-[2-(1-Adamantyl)ethyl]-3-[3-oxo-3-(4-pyridyl)propyl]-1-pentylurea

https://huagongshe.com/reaction/11488

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium SulfiteHCID 24437—
反応物TriacetoxyperiodinaneHCID 159087—
反応物Sodium BicarbonateHCID 516892—
反応物1-[2-(1-Adamantyl)ethyl]-3-[3-hydroxy-3-(4-pyridyl)propyl]-1-pentylureaHCID 21973986—
溶媒WaterHCID 962—
溶媒DichloromethaneHCID 6344—
溶媒Ethyl AcetateHCID 8857—
生成物1-[2-(1-Adamantyl)ethyl]-3-[3-oxo-3-(4-pyridyl)propyl]-1-pentylureaHCID 2197411187.8%

反応手順

1,1,1-Triacetoxy-1,1-dihydro-1,2-benziodoxol-3(1H)-one (221 mg, 0.526 mmol) was added to a solution of 1-[2-(1-adamantyl)ethyl]-3-[3-hydroxy-3-(4-pyridyl)propyl]-1-pentylurea (100 mg, 0.234 mmol) in anhydrous dichloromethane (2 ml) under ice-cooling, the temperature was raised to room temperature, and the mixture was stirred for one hour. The reaction mixture was cooled with ice again, ethyl acetate (10 ml), a saturated aqueous sodium sulfite solution (5 ml) and a saturated aqueous sodium hydrogencarbonate solution (5 ml) were added to the reaction mixture, and the whole was stirred for 15 minutes. The reaction mixture was distributed with ethyl acetate (50 ml) and water (10 ml), and the organic layer was washed with a saturated aqueous sodium sulfite solution (5 ml), a saturated aqueous sodium hydrogencarbonate solution (5 ml) and a saturated aqueous sodium chloride solution (25 ml) successively. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give 87.3 mg (87.8%) of the titled compound as colorless crystals.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07098226B2
出典データセットuspto-grants-2006_08
ORD IDord-e566d59fdc5441c397562ebe5a903995
出典メモuspto-grants-2006_08