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HRID 595040作成日:2026年10月25日

Sodium Iodide → Methyl 4-((di-tert-butoxyphosphoryloxy)methyl)benzoate

https://huagongshe.com/reaction/595040

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium IodideHCID 5238—
反応物Methyl 4-(bromomethyl)benzoateHCID 256687—
反応物Potassium di-tert-butyl phosphateHCID 23674467—
溶媒Diethyl EtherHCID 3283—
溶媒DimethylformamideHCID 6228—
生成物Methyl 4-((di-tert-butoxyphosphoryloxy)methyl)benzoateHCID 90087888—

反応手順

Methyl 4-(bromomethyl)benzoate (1200 mg, 5.24 mmol), potassium di-tert-butyl phosphate (1431 mg, 5.76 mmol) and sodium iodide (785 mg, 5.24 mmol) were combined in DMF (3.00 mL) under nitrogen. The reaction mixture was stirred at room temperature for 24 h. The reaction mixture was diluted with ether, washed with 10% LiCl solution and brine, then dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by silica gel chromatography (hexane/EtOAc) to provide Preparation 55A (571 mg, 1.593 mmol, 30%): 1H NMR (400 MHz, CDCl3) δ 8.03 (d, J=8.4 Hz, 2H), 7.53-7.37 (m, 2H), 5.05 (d, J=7.5 Hz, 2H), 3.92 (s, 3H), 1.48 (d, J=0.4 Hz, 18H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09242941B2
出典データセットuspto-grants-2016_01
ORD IDord-ddb14697f5774d0e8ba27545822bb64b
出典メモuspto-grants-2016_01