Pyridine → Dimethyl 6-amino-4-bromo-terephthalate
反応式
[NH2:1][C:2]1[CH:11]=[C:10]([C:12]([O:14][CH3:15])=[O:13])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].N1C=CC=CC=1.[Br:22]Br>ClCCl>[NH2:1][C:2]1[C:3]([C:4]([O:6][CH3:7])=[O:5])=[CH:8][CH2:9][C:10]([Br:22])([C:12]([O:14][CH3:15])=[O:13])[CH:11]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
10.5 g (50 mmol) dimethyl amino-terephthalate and 8.1 ml (100 mmol) pyridine are dissolved in 175 ml dichloromethane and at −16° C. a solution of 2.7 ml (52.5 mmol) bromine in 25 ml dichloromethane is added dropwise. It is stirred for 4 hours at 0° C. and then heated overnight to ambient temperature. The mixture is added to ice water, washed three times with water and then dried over magnesium sulphate and evaporated down. The crude product is recrystallised from ethanol.
後処理
- additionis added dropwise
- temperatureheated overnight to ambient temperature
- washwashed three times with water
- dry with materialdried over magnesium sulphate
- customevaporated down
- customThe crude product is recrystallised from ethanol
出典と根拠
- ORDレコード
- ord-a137e12451464b238fb9096e7c5a5528
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07429597B2
反応ノート
読み込み中…