Ethanol → Ethyl 5-(trifluoromethyl)-1H-pyrrolo[3,2-b]pyridine-2-carboxylate

HRID 2358165노트

반응식

HRID 2358165 반응식
S(=O)(=O)(O)O.[F:6][C:7]([F:21])([F:20])[C:8]1[N:13]=[C:12]2[CH:14]=[C:15]([C:17]([OH:19])=[O:18])[NH:16][C:11]2=[CH:10][CH:9]=1.[CH2:22](O)[CH3:23]>>[F:21][C:7]([F:6])([F:20])[C:8]1[N:13]=[C:12]2[CH:14]=[C:15]([C:17]([O:19][CH2:22][CH3:23])=[O:18])[NH:16][C:11]2=[CH:10][CH:9]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 573558695-(Trifluoromethyl)-1H-pyrrolo[3,2-b]pyridine-2-carboxylic acid

생성물 1

HCID 66811603Ethyl 5-(trifluoromethyl)-1H-pyrrolo[3,2-b]pyridine-2-carboxylate

실험 절차

1 ml (18.71 mmol) of concentrated sulfuric acid is added to a solution of 0.2 g (0.87 mmol) of 5-trifluoromethyl-pyrrolo[3,2-b]pyridine-2-carboxylic acid, obtained in step 19.2, in 10 ml of ethanol. The solution is refluxed for 20 hours and then cooled and concentrated under reduced pressure. The resulting residue is then taken up in 50 ml of dichloromethane and washed successively with 20 ml of saturated aqueous sodium hydrogen carbonate solution, 40 ml of water and 20 ml of saturated aqueous sodium chloride solution, dried over sodium sulfate and then concentrated under reduced pressure. 0.19 g of product is obtained, and is used without further purification in the following step.

후처리

  1. temperatureThe solution is refluxed for 20 hours
  2. temperaturecooled
  3. concentrationconcentrated under reduced pressure
  4. washwashed successively with 20 ml of saturated aqueous sodium hydrogen carbonate solution, 40 ml of water and 20 ml of saturated aqueous sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-fd3d76e2c89b4ef9818cbb747a2b8972
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07763636B2

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