Sulfuric Acid → HCID 86639059, 화합물

HRID 1019535노트

반응식

HRID 1019535 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>C(O)C>[F:21][C:7]([F:6])([F:20])[C:8]1[N:13]=[C:12]2[CH:14]=[CH:15][NH:16][C:11]2=[CH:10][CH:9]=1.[CH3:14][CH2:15][C:17]([O-:19])=[O:18]

참가 물질

4

반응물 2

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

생성물 1

HCID 86639059HCID 86639059, 화합물수율 168.5%

시약·촉매·용매 1

HCID 702Ethanol용매

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 Stage 10.2, in 10 mL of ethanol. It is stirred under reflux for 20 hours then the solution is cooled, and concentrated at reduced pressure. The resultant residue is then taken up in 50 mL of dichloromethane then washed successively with 20 mL of a saturated aqueous solution of sodium bicarbonate, 40 mL of water and 20 mL of saturated aqueous solution of sodium chloride, dried over sodium sulfate and then concentrated at reduced pressure. We obtain 0.19 g of product, which is used as it is in the next stage.

후처리

  1. temperatureunder reflux for 20 hours
  2. temperaturethe solution is cooled
  3. concentrationconcentrated at reduced pressure
  4. washthen washed successively with 20 mL of a saturated aqueous solution of sodium bicarbonate, 40 mL of water and 20 mL of saturated aqueous solution of sodium chloride
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated at reduced pressure

출처 및 근거

ORD 기록
ord-6c70b8815bc84e579021b42f408fe48e
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716272B2

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