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HRID 1776400作成日:2026年10月25日

Water → Benzenemethanol, 4-(difluoromethoxy)-2,6-difluoro-

https://huagongshe.com/reaction/1776400

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Cesium carbonateHCID 10796—
反応物Sodium chlorodifluoroacetateHCID 2734985—
反応物3,5-Difluoro-4-(hydroxymethyl)phenolHCID 22219975—
溶媒DimethylformamideHCID 6228—
生成物Benzenemethanol, 4-(difluoromethoxy)-2,6-difluoro-HCID 69140944—

反応条件

温度100 °C

反応手順

1 g of 3,5-difluoro-4-(hydroxymethyl)phenol (6.245 mmol, 1 eq.) were dissolved in 16 ml of DMF 1.047 g of sodium chloro(difluoro)acetate (6.87 mmol, 1.1 eq.), 2.442 g of cesium carbonate (7.494 mmol, 1.2 eq.) and 400 μl of water were added. The mixture was stirred at 100° C. bath temperature for 2 hours under nitrogen atmosphere. Then the reaction mixture was partitioned between water and ethyl acetate. The separated aqueous layer was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over a silicone filter and concentrated in vacuo. The residue was purified by flash chromatography to yield 763.3 mg (3.63 mmol, 58.2%) of the analytically pure target compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09265763B2
出典データセットuspto-grants-2016_02
ORD IDord-8bc24b5d67264f90b0e55a882efef827
出典メモuspto-grants-2016_02