2-Methoxyethanol → 4-(beta-Methoxyethoxy)-2-(beta-hydroxyethyl)amino-6-(beta-hydroxyethyl)aminonitrobenzene
反応式
Cl[C:2]1[CH:7]=[C:6]([NH:8][CH2:9][CH2:10][OH:11])[C:5]([N+:12]([O-:14])=[O:13])=[C:4]([NH:15][CH2:16][CH2:17][OH:18])[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[CH3:25][O:26][CH2:27][CH2:28][OH:29]>CN1CCCC1=O>[CH3:25][O:26][CH2:27][CH2:28][O:29][C:2]1[CH:7]=[C:6]([NH:8][CH2:9][CH2:10][OH:11])[C:5]([N+:12]([O-:14])=[O:13])=[C:4]([NH:15][CH2:16][CH2:17][OH:18])[CH:3]=1参加物
実験手順
0.09 mole (25 g) of 4-chloro-2-(β-hydroxyethyl)amino-6-(β-hydroxyethyl)aminonitrobenzene, synthesized in stage 1 of example 2, was added to a solution of 11.9 g of pelletized potash in 60 ml of 2-methoxyethanol and 25 ml of N-methylpyrrolidone and heated for 4 hours over a boiling water bath. The reaction medium was diluted with 350 ml of ice water and the desired product obtained by high pressure liquid chromatography (HPLC). About 150 ml of the aqueous solution obtained by dilution of the reaction medium were injected onto a C18RD chromatographic column (Instrument: Waters Prep 500). The desired product was eluted by a 40% methanol--60% water solution. After evaporation of the fractions containing the desired product, a dry extract was obtained which was recrystallized from isopropanol. After recrystallization, it melted at 116° C.
後処理
- temperatureheated for 4 hours over a boiling water bath
出典と根拠
- ORDレコード
- ord-924f1e9b6d5943628af752863d032451
- 出典データセット
- uspto-grants-1989_09
- 特許番号
- US04863482
反応ノート
読み込み中…