Pyridine → Dimethyl 6-amino-4-bromo-terephthalate

HRID 34142

반응식

HRID 34142 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]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 24408BromineHCID 79336Dimethyl aminoterephthalate

생성물 1

HCID 68932527Dimethyl 6-amino-4-bromo-terephthalate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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

  1. additionis added dropwise
  2. temperatureheated overnight to ambient temperature
  3. washwashed three times with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated down
  6. 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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