関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-(2,4-Dinitrophenoxy)ethanol | HCID 76070 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-(2,4-Diaminophenoxy)ethanol | HCID 47933 | 127.9% |
反応手順
A 1 l autoclave reactor was filled with 120 g of 2-(2′,4′-dinitrophenoxy)ethanol, 3 g of a 1% platinum/carbon catalyst which included 50% water, and 400 ml of isopropanol. At a hydrogen pressure of 1 MPa and a temperature of 100° C., hydrogenation was carried out for 10 h. The system was then cooled to 20° C., and the reaction mixture was added dropwise under a nitrogen atmosphere through a filter into an initial charge of 240 g of 37% strength hydrochloric acid which had been previously flushed repeatedly with nitrogen. The resulting suspension was heated at reflux temperature for about 30 min and then cooled to 10° C. The product obtained after filtration was washed once with isopropanol to give 113.1 g of 2-(2′,4′-diamino-phenoxy)ethanol (89.1% yield) in 98% purity. Measuring the degrees of transmission of a 0.1% strength solution of the product in water in accordance with DIN 55945 gave, as results, Tx=99.4, Ty=98.9 and Tz=98.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06204413B1 |
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| 出典データセット | uspto-grants-2001_03 |
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| ORD ID | ord-0043d53f073245c48ba7e87bdd1f2096 |
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| 出典メモ | uspto-grants-2001_03 |
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