Hydrogen Peroxide → 2-(3-chlorophenoxy)nicotinamide
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][CH:16]=1)[O:5][C:6]1[N:13]=[CH:12][CH:11]=[CH:10][C:7]=1[C:8]#[N:9].OO.[OH-].[K+].S([O-])([O-])(=O)=[O:22].[Mg+2]>C(O)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][CH:16]=1)[O:5][C:6]1[N:13]=[CH:12][CH:11]=[CH:10][C:7]=1[C:8]([NH2:9])=[O:22]参加物
7
反応条件
- 温度
- 0 °C
実験手順
A solution of 2-(3-Chloro-phenoxy)-nicotinonitrile (7.81 grams, 33.9 mmole), 3% hydrogen peroxide (190 ml, 169 mmole) and 50% potassium hydroxide (380 ml, 3.39 mmole) in ethanol (100 ml) was stirred at 70° C. over night. The mixture was concentrated to 250 ml and cooled to 0° C. A solid was isolated by filtration, dissolved in ethyl acetate, dired over magnesium sulfate and concentrated to a white solid (6.51 g). M.P. 225-228° C.; MW 248.67; MS (m/e) 250 (M++1).
後処理
- concentrationThe mixture was concentrated to 250 ml
- customA solid was isolated by filtration
- concentrationconcentrated to a white solid (6.51 g)
出典と根拠
- ORDレコード
- ord-96f39733c9594f15b295688aee3311b4
- 出典データセット
- uspto-grants-2002_04
- 特許番号
- US06380218B1
反応ノート
読み込み中…