Methyl morpholine oxide → [4-(4-Chlorophenoxy)-2-propylphenyl][4-chloro-2-fluoro-5-methoxyphenyl]methanone

関与物質

役割	名称	HCID	仕込み量
反応物	Methyl morpholine oxide	HCID 82029	—
反応物	Tetrabutylammonium Fluoride	HCID 2724141	—
反応物	[4-Chloro-2-fluoro-5-methoxy-3-(trimethylsilyl)phenyl][4-(4-chlorophenoxy)-2-propylphenyl]methanol	HCID 86622409	—
触媒	HCID 178419074	HCID 178419074	—
溶媒	Diethyl Ether	HCID 3283	—
溶媒	Dichloromethane	HCID 6344	—
溶媒	Tetrahydrofuran	HCID 8028	—
溶媒	Ethyl Acetate	HCID 8857	—
生成物	[4-(4-Chlorophenoxy)-2-propylphenyl][4-chloro-2-fluoro-5-methoxyphenyl]methanone	HCID 68689947	—

反応条件

温度	25 °C

反応手順

A mixture of the product from Step 2 (1.9 g, 3.7 mmol), N-methylmorpholine-N-oxide (0.70 g, 6.0 mmol), tetrapropylammonium perruthenate (70 mg, 0.2 mmol) and 4 Å molecular sieves (2.0 g) in dichloromethane (20 mL) was stirred at 25° C. for 1 h. The reaction mixture was diluted with diethyl ether (60 mL) and filtered through a short path of silica gel. Removal of the solvent gave the crude product. The crude product was dissolved in THF (20 mL) and treated with tetrabutylammonium fluoride (1M in THF, 5.6 mL, 5.6 mmol) for 10 min. The reaction mixture was diluted with ethyl acetate, washed with brine, dried and concentrated. The residue was purified by chromatography on silica gel to give the title product.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07834036B2
出典データセット	uspto-grants-2010_11
ORD ID	ord-b99a6ec23c2e45b0893015d613d683f8
出典メモ	uspto-grants-2010_11