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HRID 1516024作成日:2026年10月26日

Lithium hydroxide, monohydrate → (7-Methoxymethoxymethyl-1,1-dioxo-1,4-dihydro-1lambda6-thieno[2,3-e][1,2,4]thiadiazin-3-yl)-acetic acid

https://huagongshe.com/reaction/1516024

反応式

関与物質

役割名称HCID仕込み量
反応物Lithium hydroxide, monohydrateHCID 168937—
反応物(7-Methoxymethoxymethyl-1,1-dioxo-1,4-dihydro-1lambda6-thieno[2,3-e][1,2,4]thiadiazin-3-yl)-acetic acid ethyl esterHCID 58000246—
溶媒WaterHCID 962—
溶媒TetrahydrofuranHCID 8028—
生成物(7-Methoxymethoxymethyl-1,1-dioxo-1,4-dihydro-1lambda6-thieno[2,3-e][1,2,4]thiadiazin-3-yl)-acetic acidHCID 5800026978.1%

反応条件

温度25 °C

反応手順

To a solution of (7-methoxymethoxymethyl-1,1-dioxo-1,4-dihydro-1λ6-thieno[2,3-e][1,2,4]thiadiazin-3-yl)-acetic acid ethyl ester (0.54 g, 1.55 mmol) in tetrahydrofuran (5 mL) and water (5 mL) was added lithium hydroxide monohydrate (0.33 g, 7.75 mmol). The reaction was stirred at 25° C. for 1 h before it was cooled to 0° C. The reaction was quenched via the addition of 6.0 M aqueous hydrochloric acid solution until a pH of 1-2 was reached. The resulting mixture was extracted with ethyl acetate (3×10 mL). The organic layers were combined, dried over magnesium sulfate, filtered and concentrated in vacuo to afford the crude product, (7-methoxymethoxymethyl-1,1-dioxo-1,4-dihydro-1λ6-thieno[2,3-e][1,2,4]thiadiazin-3-yl)-acetic acid (0.39 g, 1.21 mmol, 78%), which was used in the next step without further purification.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08222404B2
出典データセットuspto-grants-2012_07
ORD IDord-ea8560ccdbbd410f92f3e5c03150c0af
出典メモuspto-grants-2012_07