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Water → 4-Chloro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Chloro-5-(5-isoquinolylsulfanyl)-2-nitroaniline | HCID 21846903 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 4-Chloro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine | HCID 21846930 | 89.5% |
反応手順
4-Chloro-5-(5-isoquinolylsulfanyl)-2-nitroaniline 1.78 g (5.4 mmol) was dissolved in concentrated hydrochloric acid 30 ml, stannous chloride dihydrate 4.30 g (19.1 mmol) was added, and the mixture was stirred overnight at room temperature. The reaction mixture was poured into water, 50% sodium hydroxide was added to alkalize the mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and with saturated sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was recrystallized from ethyl acetate-n-hexane to give 4-chloro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine 1.45 g (89.5%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05959107 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-064ef837141c4fd78d5569ce18e1284f |
| 出典メモ | uspto-grants-1999_09 |