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

HRID 34142

反応式

HRID 34142 の反応式
[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

反応物 3

HCID 1049PyridineHCID 24408BromineHCID 79336Dimethyl aminoterephthalate

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

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

  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

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

関連ノート

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