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HRID 241519作成日:2026年10月26日

Water → 4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzimidic acid methyl ester

https://huagongshe.com/reaction/241519

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Methyl iodideHCID 6328—
反応物Cesium carbonateHCID 10796—
反応物4-bromo-3-chloro-N-trimethylsilanylmethylthiobenzamideHCID 86685705—
溶媒TetrahydrofuranHCID 8028—
生成物4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzimidic acid methyl esterHCID 6683665976.2%

反応条件

温度40 °C

反応手順

To a solution of 4-bromo-3-chloro-N-trimethylsilanylmethyl-thiobenzamide (10.40 g, 30.88 mmol) in THF (200 mL) was added methyl iodide (5.77 mL, 13.15 g, 92.7 mmol) and Cs2CO3 (30.19 g, 92.7 mmol) at −5° C. After 1 h at this temperature, the mixture was heated at 40° C. and stirred over night. Water was added and the mixture was extracted three times with MTBE. The combined organic phases were dried over Na2SO4, filtered and concentrated in vacuum. The residue was purified by filtration over a short plug of silica gel to give the title compound (8.25 g), 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US08653000B2
出典データセットuspto-grants-2014_02
ORD IDord-c293342cb2f44c8c9470e59173be86d6
出典メモuspto-grants-2014_02