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HRID 1398857作成日:2026年10月25日

Thiophosgene → 5-Isothiocyanato-2-methoxy-4-methylpyridine

https://huagongshe.com/reaction/1398857

反応式

関与物質

役割名称HCID仕込み量
反応物ThiophosgeneHCID 10040—
反応物6-Methoxy-4-methylpyridin-3-amineHCID 243170—
溶媒TetrahydrofuranHCID 8028—
溶媒Sodium BicarbonateHCID 516892—
生成物5-Isothiocyanato-2-methoxy-4-methylpyridineHCID 8663288459%

反応条件

温度0 °C

反応手順

Thiophosgene (8.9 mL, 120 mmol) was added dropwise to a stirred mixture of 6-methoxy-4-methylpyridin-3-amine (13.8 g, 99.8 mmol) in tetrahydrofuran (100 mL) and saturated aqueous sodium hydrogen carbonate (150 mL) at 0° C., and the mixture was stirred at 0° C. for 2 hr. The mixture was diluted with saturated aqueous sodium hydrogen carbonate, and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was washed with n-hexane to give the title compound as a colorless powder (10.6 g, 58.8 mmol, 59%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08901141B2
出典データセットuspto-grants-2014_12
ORD IDord-d17bc03c4b95426fba488b1b021ca0ff
出典メモuspto-grants-2014_12