Pyridine → Dimethyl 6-amino-4-bromo-terephthalate
반응식
[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]=1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-a137e12451464b238fb9096e7c5a5528
- 출처 데이터셋
- uspto-grants-2008_09
- 특허 번호
- US07429597B2
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