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HRID 1036404作成日:2026年10月26日

Ethanol → HCID 178464723、化合物

https://huagongshe.com/reaction/1036404

反応式

関与物質

役割名称HCID仕込み量
反応物EthanolHCID 702—
反応物Lithium hydroxide, monohydrateHCID 168937—
反応物HCID 178421574HCID 178421574—
溶媒WaterHCID 962—
生成物HCID 178464723HCID 1784647236%

反応条件

温度80 °C

反応手順

To a solution of (R)-4-Methyl-4-[6-(cis4-methyl-cyclohexyloxy)-naphthalen-2-yl]-oxazolidin-2-one (0.4420 g, 0.001302 mol) in ethanol (5.00 mL, 0.0856 mol) in a capped 40 mL vial was added 4.2 M Lithium hydroxide, monohydrate in water (2.8 mL). The mixture was heated overnight at 80° C. TLC analysis showed the reaction was complete. The mixture was concentrated to dryness under vacuum. Methylene chloride (5 mL) and water (5 mL) were added and the layers were separated (2×). The organic layer was concentrated under vacuum and purified by HPLC to give 0.0233 g of the title compound (6% yield). MS: m/z=297.29 [M−NH2]+. 1H NMR (400 MHz, MeOD) δ 0.98 (d, J=6.02 Hz, 3H), 1.40-1.51 (m, 2H), 1.51-1.60 (m, 3H), 1.64-1.74 (m, 2H), 1.79 (s, 3H), 2.03-2.14 (m, 2H), 3.83 (d, J=11.55 Hz, 1H), 3.93 (d, J=11.55 Hz, 1H), 4.69-4.77 (m, 1H), 7.23 (dd, J=8.91, 2.38 Hz, 1H), 7.27 (d, J=2.51 Hz, 1H), 7.53 (dd, J=8.78, 2.01 Hz, 1H), 7.79-7.89 (m, 3H)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08546359B2
出典データセットuspto-grants-2013_10
ORD IDord-e4605061053247c280ea13972fb55ad0
出典メモuspto-grants-2013_10