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Water → 3,5-Dichloro-3-(2-methoxyphenyl)indolin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 5-Chloro-3-hydroxy-3-(2-methoxyphenyl)indolin-2-one | HCID 21905955 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3,5-Dichloro-3-(2-methoxyphenyl)indolin-2-one | HCID 21905913 | — |
反応手順
38 ml (0.518 mol) thionyl chloride were slowly added by drops to 100 g (0.345 mol) of the intermediate product 1a, 56 ml (0.695 mol) pyridine in 1 l methylene chloride at 0° C., and then stirred for approximately 30 minutes more. Then the reaction mixture was poured on to icy water and the organic phase was separated. This organic phase was then washed with water, dried and concentrated in a vacuum. The residue was treated with toluene a number of times and the organic solvent was removed in a vacuum each time. 79 g of the raw product were obtained and further reacted without further cleaning.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07951807B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-6fd1ca05de294db6a5c76e158bcc37e6 |
| 出典メモ | uspto-grants-2011_05 |