関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Sodium chlorodifluoroacetate | HCID 2734985 | — |
| 反応物 | 3,5-Difluoro-4-(hydroxymethyl)phenol | HCID 22219975 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzenemethanol, 4-(difluoromethoxy)-2,6-difluoro- | HCID 69140944 | — |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09265763B2 |
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| 出典データセット | uspto-grants-2016_02 |
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| ORD ID | ord-8bc24b5d67264f90b0e55a882efef827 |
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| 出典メモ | uspto-grants-2016_02 |
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