反応式
[N+:1]([C:4]1[CH:13]=[C:12]([N+:14]([O-])=O)[CH:11]=[CH:10][C:5]=1[O:6][CH2:7][CH2:8][OH:9])([O-])=O.O.[H][H]>[Pt].C(O)(C)C>[NH2:1][C:4]1[CH:13]=[C:12]([NH2:14])[CH:11]=[CH:10][C:5]=1[O:6][CH2:7][CH2:8][OH:9]参加物
反応条件
- 温度
- 20 °C
実験手順
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.
後処理
- additionthe reaction mixture was added dropwise under a nitrogen atmosphere through
- filtrationa filter into
- additionan initial charge of 240 g of 37% strength hydrochloric acid which
- customhad been previously flushed repeatedly with nitrogen
- temperatureThe resulting suspension was heated
- temperatureat reflux temperature for about 30 min
- temperaturecooled to 10° C
- customThe product obtained
- filtrationafter filtration
- washwas washed once with isopropanol
出典と根拠
- ORDレコード
- ord-0043d53f073245c48ba7e87bdd1f2096
- 出典データセット
- uspto-grants-2001_03
- 特許番号
- US06204413B1
関連ノート
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