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Water → 1-(3,4-Dichlorobenzyl)-2-(2-hydroxy-5-nitrobenzyl)-5-methylthio-1,2-dihydroindazol-3-one hydrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(Chloromethyl)-4-nitrophenol | HCID 76305 | — |
| 反応物 | HCID 178503082 | HCID 178503082 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(3,4-Dichlorobenzyl)-2-(2-hydroxy-5-nitrobenzyl)-5-methylthio-1,2-dihydroindazol-3-one hydrate | HCID 21262705 | — |
反応手順
3.6 g (11 mmol) of 1-(3,4-dichlorobenzyl)-5-methylthio-1H-indazol-3-ol are dissolved in 100 ml of DMSO and treated in portions with 0.34 g (13.2 mmol) of sodium hydride (95 percent). After stirring for 2 hours, a solution of 2.1 g (11 mmol) of 2-hydroxy-5-nitrobenzyl chloride in 20 ml of DMSO is added dropwise and the mixture is stirred at 60° C. for 3 hours. After cooling, 200 ml of water are added dropwise, the mixture is stirred for 4 hours and the solid is filtered off with suction. The precipitate is extracted by stirring with methanol whilst hot and recrystallized from 2-propanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06180637B2 |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-0dc3658d526748e18bebe64c0ad5583e |
| 出典メモ | uspto-grants-2001_01 |