関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bicarbonate Ion | HCID 769 | — |
| 反応物 | N-(2,2-dimethoxyethyl)-N-methanesulphonyl-4-fluoro-3-methoxyaniline | HCID 22570034 | — |
| 触媒 | Titanium Tetrachloride | HCID 24193 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 5-Fluoro-1-methanesulphonyl-6-methoxyindole | HCID 22570050 | — |
反応手順
To a solution of N-(2,2-dimethoxyethyl)-N-methanesulphonyl-4-fluoro-3-methoxyaniline (1.91 g, 0.65 mmol) in dry toluene at 0° C. under argon, was added slowly a solution of TiCl4 (0.173 g, 0.911 mmol) in dry toluene (10 ml). The solution was then heated to 70° C. for 1 h. cooled and poured onto ice/sat. sod. bicarbonate solution (20 ml). The organic layer was separated, washed with sat. sod. bicarbonate solution, 0.5% hydrochloric acid (2×20 ml) and water (2×20 ml). The solution was dried (MgSO4) and evaporated in vacuo to give 5-fluoro-1-methanesulphonyl-6-methoxyindole ((0.102 g)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06855715B1 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-ab5cf9bb3daa461ab50b0a25299f6c60 |
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| 出典メモ | uspto-grants-2005_02 |
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