2-Chloroethanol → 2-(2-Nitrophenoxy)ethanol
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10])([O-:3])=[O:2].[OH-].[Na+].O.Cl[CH2:15][CH2:16][OH:17]>C(O)CCC>[OH:17][CH2:16][CH2:15][O:10][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[N+:1]([O-:3])=[O:2]参加物
6
反応条件
- 温度
- 100 °C
実験手順
10 g (71.88 mmol) 2-nitrophenol A1 and 3.59 g (89.86 mmol) sodium hydroxide were dissolved in 55 ml n-butanol and 5 ml water at 70° C., 6.26 ml (7.52 g, 93.44 mmol) 2-chloroethanol were slowly added drop by drop. This was followed by three days of vigorous stirring at 100° C. After cooling, the reaction mixture was filtrated, the precipitate washed with chloroform and the filtrate reduced. The residue was taken up in chloroform and washed three times with aqueous 10% sodium hydroxide solution. Then the organic phase was dried over sodium sulfate and was concentrated in vacuo. 10.8 g of bright yellow crystals were obtained; yield 82%.
後処理
- customat 70° C.
- temperatureAfter cooling
- filtrationthe reaction mixture was filtrated
- washthe precipitate washed with chloroform
- washwashed three times with aqueous 10% sodium hydroxide solution
- dry with materialThen the organic phase was dried over sodium sulfate
- concentrationwas concentrated in vacuo
出典と根拠
- ORDレコード
- ord-0e9a22ae3ae24416ad7ab933bafa35b7
- 出典データセット
- uspto-grants-2000_09
- 特許番号
- US06124135
反応ノート
読み込み中…