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Hydrochloric Acid → 7,8-Diamino-1-hydroxy-3-naphthalene sulfonic acid dihydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Amino-8-hydroxynaphthalene-6-sulfonic acid | HCID 7022 | — |
| 反応物 | Sodium Dithionite | HCID 24489 | — |
| 反応物 | Sodium sulfanilate | HCID 23664644 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 7,8-Diamino-1-hydroxy-3-naphthalene sulfonic acid dihydrochloride | HCID 87885844 | 45% |
反応手順
A stirred solution of p-benzenediazonium sulfonic acid, was prepared by the addition of sodium sulfanilate (1.10 g, 5.2 mmole) to sodium nitrite (0.40 g, 5.7 mmole) in water (10 mL) followed by addition to ice (6.0 g) and concentrated HCl (1.1 mL, 37%). After 30 min. of standing at 0° C. 7-amino-1-hydroxy-3-naphthalene sulfonic acid (1.2 g, 5.2 mmole) was added in water (10 mL) and the reaction was stirred at room temperature overnight. The reaction mixture was warmed to 50° C. and sodium hydrosulfite (3.0 g, 15.6 mmole) was added and the reaction was stirred for 4 hours. The reaction was filtered and the precipitate was washed with water, methanol, and ether to give the title compound (0.54 g; 45%) as a red solid. MS(ES) m/z 255 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858630B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-f48772335f1d4b98924d18b5e0cf3276 |
| 出典メモ | uspto-grants-2005_02 |