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Potassium Carbonate → HCID 21911050、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzoic acid, 2-fluoro-, ethyl ester | HCID 67953 | — |
| 反応物 | Tert-butyl(4'-hydroxybiphenyl-3-ylmethyl)methylcarbamate | HCID 69643261 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | HCID 21911050 | HCID 21911050 | 104.9% |
反応手順
2.15 g (12.8 mmol) of ethyl 2-fluorobenzoate and 1.9 g (14 mmol) of potassium carbonate are successively added to a solution of 4 g (12.8 mmol) of tert-butyl (4′-hydroxybiphenyl-3-ylmethyl)methylcarbamate in 45 ml of dimethylacetamide. The reaction medium is refluxed for 48 hours, cooled, diluted with water and extracted with ethyl acetate. The organic phase is dried over sodium sulfate, filtered and concentrated under vacuum. The residue obtained is purified by chromatography on a column of silica eluted with an 80/20 heptane/ethyl acetate mixture. 3.1 g of ethyl 2-{3′-[(tert-butoxycarbonylmethylamino)methyl]biphenyl-4-yloxy}benzoate are obtained in the form of a colorless oil, in a yield of 53%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07307078B2 |
| 出典データセット | uspto-grants-2007_12 |
| ORD ID | ord-cb2bf88750c64ea8856627e28cf92620 |
| 出典メモ | uspto-grants-2007_12 |