関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | indium(III)chloride | HCID 159675 | — |
| 反応物 | (4-Chlorophenyl)(4-fluorophenyl)methanol | HCID 12634874 | — |
| 反応物 | 3-(2,4-Dichlorophenyl)-3-{5-fluoro-7-[(methylsulfanyl)methyl]-1H-indol-3-yl}propan-1-ol | HCID 58392305 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-[(4-Chlorophenyl)(4-fluorophenyl)methyl]-7-[(methylsulfanyl)methyl]-1H-indole | HCID 58392203 | — |
反応手順
2.94 g (12.41 mmol) of the compound from Example 81A and 2.50 g (11.28 mmol) of indium(III) chloride were added to 2.00 g (11.28 mmol) of the compound from Example 8 in 100 ml of toluene. The reaction mixture was stirred at 80° C. for 3 h. After cooling to RT, the reaction solution was mixed with water and ethyl acetate and the solid was filtered off. The phases of the filtrate were separated, and the aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated. Purification of the crude product by preparative HPLC (mobile phase: acetonitrile/water gradient) resulted in 0.83 g (19% of theory) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08063234B2 |
|---|
| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-f82843f8ab13408c9b2b316e0f3d0001 |
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| 出典メモ | uspto-grants-2011_11 |
|---|
