関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,4-Bis(1-methyl-1-phenylethyl)-6-[2-(2-nitrophenyl)diazenyl]phenol | HCID 116810 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-(2H-Benzotriazol-2-yl)-4,6-bis(1-methyl-1-phenylethyl)phenol | HCID 112412 | — |
反応手順
To a 5-liter 3-necked flask fitted with a stirrer, thermometer, reflux condenser and nitrogen inlet was charged 386 grams (0.805 mol) of the o-nitroazobenzene intermediate of Example 2 and 1200 ml of toluene. To the resulting solution was added 240 ml of isopropanol and 240 ml of water. A nitrogen atmosphere was imposed and 160 ml of 50.15 aqueous sodium hydroxide was added. A flask containing 158.2 grams (2.42 gram-atoms) of zinc was connected to the reaction flask by Gooch rubber tubing and the zinc dust was added portionwise to the reaction mixture over a 90-minute period. The zinc was added at such a rate to keep the internal temperature between 40° and 45° C. After the zinc was all added, the reaction mixture was heated for 1 hour at 40° C. and then for 3 hours at 70° C. The mixture was cooled to room temperature and acidified with 600 ml of concentrated hydrochloric acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04275004 |
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| 出典データセット | uspto-grants-1981_06 |
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| ORD ID | ord-ff220221845e425989c9b5d57f14220d |
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| 出典メモ | uspto-grants-1981_06 |
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