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HRID 1161028作成日:2026年10月24日

Methanol → HCID 66699549、化合物

https://huagongshe.com/ja/reaction/1161028

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物DichloromethaneHCID 6344—
反応物p-Toluenesulfonic acid monohydrateHCID 521998—
反応物3-[[4-(4-Acetyl-3-hydroxy-2-propyl-phenoxymethyl)-phenyl]-(tetrahydro-pyran-2-yloxy)-methyl]-benzonitrileHCID 66699604—
溶媒Ethyl AcetateHCID 8857—
生成物HCID 66699549HCID 6669954993%

反応条件

温度0 °C

反応手順

Stir a mixture of 3-[[4-(4-acetyl-3-hydroxy-2-propyl-phenoxymethyl)-phenyl]-(tetrahydro-pyran-2-yloxy)-methyl]-benzonitrile (13.4 g, 26.88 mmol), p-toluenesulfonic acid monohydrate (5.1 g, 26.88 mmol), methanol (100 mL), dichloromethane (50 mL), and ethyl acetate (50 mL) at room temperature for an hour. Concentrate the reaction mixture, dilute with ethyl acetate (150 mL) and wash with water (2×100 mL). Dry the organic phase over magnesium sulfate, filter, and concentrate. Dilute the residue with 5:1 hexanes:dichloromethane (50 mL), cool to 0° C. and filter. Collect a second and third crop to give the title compound (10.3 g, 93%), as a white solid. LCMS 416 M+1.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07816523B2
出典データセットuspto-grants-2010_10
ORD IDord-faddbb6ac0d644f8850447eac37b3f1d
出典メモuspto-grants-2010_10