関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,6-Dioxaspiro[2.5]octane | HCID 160439 | — |
| 反応物 | (1S,2S)-2-{4-[(R)-4-(4-Hydroxy-phenyl)-5-trifluoromethyl-indan-1-yloxy]-phenyl}-cyclopropanecarboxylic acid ethyl ester | HCID 86703894 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 86703895 | HCID 86703895 | — |
反応手順
((1S,2S)-2-{4-[(R)-4-(4-Hydroxy-phenyl)-5-trifluoromethyl-indan-1-yloxy]-phenyl}-cyclopro-panecarboxylic acid ethyl ester (crude from step 2), 1,6-dioxa-spiro[2.5]octane (US2012/46304, 44 mg) and cesium carbonate (198 mg) are suspended in dry N,N-dimethylformamide and heated at 100° C. for 3 hours. The mixture is diluted with water, acidified with 0.2 M HCl solution and extracted with ethyl acetate. The combined organic extracts are concentrated under vacuum and the residue purified by flash chromatography (0-30% EtOAc in cyclohexane) ti give the title compound (yield 50 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08633182B2 |
|---|
| 出典データセット | uspto-grants-2014_01 |
|---|
| ORD ID | ord-2ef9da7c07234a1bbac33a7b94f0ad9d |
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| 出典メモ | uspto-grants-2014_01 |
|---|
