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HRID 249724作成日:2026年10月26日

Methyl iodide → 1-Bromo-5-(1,1-dimethoxyethyl)-2-methoxy-3-trifluoromethylbenzene

https://huagongshe.com/reaction/249724

反応式

関与物質

役割名称HCID仕込み量
反応物Methyl iodideHCID 6328—
反応物Trimethyl orthoformateHCID 9005—
反応物Potassium CarbonateHCID 11430—
反応物3'-Bromo-4'-hydroxy-5'-(trifluoromethyl)acetophenoneHCID 58085700—
触媒D-Camphorsulfonic AcidHCID 65617—
溶媒MethanolHCID 887—
溶媒DimethylformamideHCID 6228—
溶媒Heptane waterHCID 57468513—
生成物1-Bromo-5-(1,1-dimethoxyethyl)-2-methoxy-3-trifluoromethylbenzeneHCID 58085697—

反応手順

1-(3-Bromo-4-hydroxy-5-trifluoromethylphenyl)ethanone (6.8 g) was dissolved in absolute methanol (50 ml) and treated successively with DL-10-camphorsulfonic acid (111 mg) and trimethyl orthoformate (8 ml). After stirring at RT for 2 h, DMF (75 ml) and potassium carbonate (5.0 g) were added, followed by iodomethane (3 ml). After stirring for 6 h, the batch was allowed to stand overnight and was treated with a 1:1 mixture of n-heptane/water. After separating off the organic phase, it was additionally extracted once with n-heptane and then the combined heptane phases were dried over magnesium sulfate, filtered and concentrated. 7 g of the desired product were obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07863269B2
出典データセットuspto-grants-2011_01
ORD IDord-d7babac152f64052b75fdb5119acece3
出典メモuspto-grants-2011_01